# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Balakrishna, Maravanji' _publ_contact_author_address ; ; _publ_contact_author_email krishna@chem.iitb.ac.in _publ_author_name M.Balakrishna # Attachment '- MSB-94.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 779798' #TrackingRef '- MSB-94.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3-Di-tert-butyl-2,4-bis(2-diphenylphosphanyl- phenoxy)-[1,3,2,4]diazdiphosphetidine ; _chemical_name_common ; 1,3-Di-tert-butyl-2,4-bis(2-diphenylphosphanyl-phenoxy)- (1,3,2,4)diazdiphosphetidine ; _chemical_melting_point ? _chemical_formula_moiety 'C44 H46 N2 O2 P4' _chemical_formula_sum 'C44 H46 N2 O2 P4' _chemical_formula_weight 758.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.0077(8) _cell_length_b 29.659(3) _cell_length_c 15.362(1) _cell_angle_alpha 90.00 _cell_angle_beta 104.984(1) _cell_angle_gamma 90.00 _cell_volume 3964.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5821 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.85 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9334 _exptl_absorpt_correction_T_max 0.9947 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames (0.3 deg. width in omega) at phi = 0, 120 and 240 deg. A scan time of 50 sec/frame was used. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34965 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.75 _reflns_number_total 17354 _reflns_number_gt 13548 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SMART (Bruker-AXS, 2000)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. ; _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. The crystal proved, on refinement, to be a racemic twin. ; _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^)+(0.0527P)^2^] 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_abs_structure_details ; From the value determined for the Flack parameter (Flack H D (1983), Acta Cryst. A39, 876-881), the crystal was shown to be a racemic twin. ; _refine_ls_abs_structure_Flack 0.31(7) _refine_ls_number_reflns 17354 _refine_ls_number_parameters 950 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 P1 P 0.78612(10) 0.51937(3) 0.56574(6) 0.01593(19) Uani 1 1 d . . . P2 P 1.06188(10) 0.55446(3) 0.36911(6) 0.01503(19) Uani 1 1 d . . . P3 P 0.95404(10) 0.51637(3) 0.21481(6) 0.01580(19) Uani 1 1 d . . . P4 P 0.51028(11) 0.52195(3) 0.02772(6) 0.0176(2) Uani 1 1 d . . . O1 O 0.7701(3) 0.50042(8) 0.18300(15) 0.0173(5) Uani 1 1 d . . . O2 O 0.9402(3) 0.55794(9) 0.43406(15) 0.0184(6) Uani 1 1 d . . . N1 N 0.9555(3) 0.56828(10) 0.26322(19) 0.0164(7) Uani 1 1 d . . . N2 N 1.0272(3) 0.50172(10) 0.32575(19) 0.0153(6) Uani 1 1 d . . . C1 C 0.6632(4) 0.52992(12) 0.6429(2) 0.0151(8) Uani 1 1 d . . . C2 C 0.7008(4) 0.51894(13) 0.7333(2) 0.0191(8) Uani 1 1 d . . . H2 H 0.7979 0.5057 0.7601 0.023 Uiso 1 1 calc R . . C3 C 0.5997(5) 0.52687(13) 0.7855(3) 0.0235(9) Uani 1 1 d . . . H3 H 0.6282 0.5193 0.8477 0.028 Uiso 1 1 calc R . . C4 C 0.4581(5) 0.54567(13) 0.7480(3) 0.0255(9) Uani 1 1 d . . . H4 H 0.3889 0.5510 0.7842 0.031 Uiso 1 1 calc R . . C5 C 0.4167(5) 0.55680(15) 0.6578(3) 0.0272(9) Uani 1 1 d . . . H5 H 0.3187 0.5697 0.6318 0.033 Uiso 1 1 calc R . . C6 C 0.5179(4) 0.54916(13) 0.6051(3) 0.0223(8) Uani 1 1 d . . . H6 H 0.4890 0.5570 0.5430 0.027 Uiso 1 1 calc R . . C7 C 0.9207(4) 0.47759(13) 0.6304(2) 0.0163(8) Uani 1 1 d . . . C8 C 1.0651(4) 0.48761(13) 0.6866(2) 0.0220(8) Uani 1 1 d . . . H8 H 1.0974 0.5182 0.6949 0.026 Uiso 1 1 calc R . . C9 C 1.1624(5) 0.45381(14) 0.7305(3) 0.0274(10) Uani 1 1 d . . . H9 H 1.2601 0.4612 0.7689 0.033 Uiso 1 1 calc R . . C10 C 1.1164(5) 0.40901(14) 0.7182(3) 0.0269(9) Uani 1 1 d . . . H10 H 1.1828 0.3856 0.7476 0.032 Uiso 1 1 calc R . . C11 C 0.9724(5) 0.39864(14) 0.6624(3) 0.0250(9) Uani 1 1 d . . . H11 H 0.9398 0.3681 0.6540 0.030 Uiso 1 1 calc R . . C12 C 0.8767(4) 0.43291(13) 0.6193(3) 0.0217(9) Uani 1 1 d . . . H12 H 0.7787 0.4255 0.5812 0.026 Uiso 1 1 calc R . . C13 C 0.9036(4) 0.57132(12) 0.5799(2) 0.0156(7) Uani 1 1 d . . . C14 C 0.9293(4) 0.59823(13) 0.6560(2) 0.0213(8) Uani 1 1 d . . . H14 H 0.8877 0.5894 0.7043 0.026 Uiso 1 1 calc R . . C15 C 1.0144(5) 0.63784(13) 0.6635(3) 0.0238(9) Uani 1 1 d . . . H15 H 1.0323 0.6555 0.7168 0.029 Uiso 1 1 calc R . . C16 C 1.0731(4) 0.65124(13) 0.5925(2) 0.0207(8) Uani 1 1 d . . . H16 H 1.1302 0.6785 0.5967 0.025 Uiso 1 1 calc R . . C17 C 1.0487(4) 0.62511(13) 0.5159(2) 0.0192(8) Uani 1 1 d . . . H17 H 1.0882 0.6345 0.4671 0.023 Uiso 1 1 calc R . . C18 C 0.9662(4) 0.58486(12) 0.5097(2) 0.0158(8) Uani 1 1 d . . . C19 C 0.9299(4) 0.61348(13) 0.2207(2) 0.0208(8) Uani 1 1 d . . . C20 C 0.8168(5) 0.63916(15) 0.2626(3) 0.0336(11) Uani 1 1 d . . . H20A H 0.7152 0.6250 0.2439 0.050 Uiso 1 1 calc R . . H20B H 0.8095 0.6706 0.2422 0.050 Uiso 1 1 calc R . . H20C H 0.8537 0.6383 0.3285 0.050 Uiso 1 1 calc R . . C21 C 1.0799(5) 0.63943(13) 0.2374(3) 0.0272(9) Uani 1 1 d . . . H21A H 1.1270 0.6413 0.3024 0.041 Uiso 1 1 calc R . . H21B H 1.0595 0.6699 0.2125 0.041 Uiso 1 1 calc R . . H21C H 1.1499 0.6238 0.2081 0.041 Uiso 1 1 calc R . . C22 C 0.8612(6) 0.60813(15) 0.1200(3) 0.0368(11) Uani 1 1 d . . . H22A H 0.9346 0.5924 0.0934 0.055 Uiso 1 1 calc R . . H22B H 0.8387 0.6379 0.0922 0.055 Uiso 1 1 calc R . . H22C H 0.7660 0.5906 0.1094 0.055 Uiso 1 1 calc R . . C23 C 1.0979(4) 0.45826(12) 0.3648(2) 0.0163(8) Uani 1 1 d . . . C24 C 1.2658(4) 0.46564(14) 0.4147(3) 0.0284(9) Uani 1 1 d . . . H24A H 1.3225 0.4765 0.3724 0.043 Uiso 1 1 calc R . . H24B H 1.3105 0.4371 0.4414 0.043 Uiso 1 1 calc R . . H24C H 1.2723 0.4880 0.4625 0.043 Uiso 1 1 calc R . . C25 C 1.0101(5) 0.44154(13) 0.4301(3) 0.0285(9) Uani 1 1 d . . . H25A H 1.0274 0.4620 0.4818 0.043 Uiso 1 1 calc R . . H25B H 1.0459 0.4112 0.4509 0.043 Uiso 1 1 calc R . . H25C H 0.9001 0.4405 0.3998 0.043 Uiso 1 1 calc R . . C26 C 1.0857(5) 0.42476(13) 0.2886(3) 0.0258(9) Uani 1 1 d . . . H26A H 0.9777 0.4214 0.2553 0.039 Uiso 1 1 calc R . . H26B H 1.1263 0.3955 0.3135 0.039 Uiso 1 1 calc R . . H26C H 1.1452 0.4358 0.2478 0.039 Uiso 1 1 calc R . . C27 C 0.6476(4) 0.51715(13) 0.2130(2) 0.0166(7) Uani 1 1 d . . . C28 C 0.6543(4) 0.51879(14) 0.3035(2) 0.0182(8) Uani 1 1 d . . . H28 H 0.7425 0.5080 0.3468 0.022 Uiso 1 1 calc R . . C29 C 0.5303(4) 0.53643(13) 0.3310(2) 0.0196(8) Uani 1 1 d . . . H29 H 0.5343 0.5381 0.3933 0.024 Uiso 1 1 calc R . . C30 C 0.4015(4) 0.55147(13) 0.2676(2) 0.0215(8) Uani 1 1 d . . . H30 H 0.3178 0.5640 0.2864 0.026 Uiso 1 1 calc R . . C31 C 0.3945(4) 0.54833(13) 0.1768(2) 0.0180(8) Uani 1 1 d . . . H31 H 0.3045 0.5582 0.1337 0.022 Uiso 1 1 calc R . . C32 C 0.5171(4) 0.53094(12) 0.1470(2) 0.0152(8) Uani 1 1 d . . . C33 C 0.3284(4) 0.55111(13) -0.0242(2) 0.0210(8) Uani 1 1 d . . . C34 C 0.3344(5) 0.59807(13) -0.0318(3) 0.0279(9) Uani 1 1 d . . . H34 H 0.4309 0.6129 -0.0140 0.034 Uiso 1 1 calc R . . C35 C 0.2038(5) 0.62303(14) -0.0644(3) 0.0338(10) Uani 1 1 d . . . H35 H 0.2109 0.6549 -0.0683 0.041 Uiso 1 1 calc R . . C36 C 0.0632(5) 0.60250(15) -0.0915(3) 0.0349(11) Uani 1 1 d . . . H36 H -0.0272 0.6199 -0.1136 0.042 Uiso 1 1 calc R . . C37 C 0.0546(5) 0.55600(17) -0.0861(3) 0.0383(11) Uani 1 1 d . . . H37 H -0.0423 0.5414 -0.1057 0.046 Uiso 1 1 calc R . . C38 C 0.1857(4) 0.53055(14) -0.0525(3) 0.0292(10) Uani 1 1 d . . . H38 H 0.1779 0.4987 -0.0488 0.035 Uiso 1 1 calc R . . C39 C 0.4506(4) 0.46288(13) 0.0158(2) 0.0178(8) Uani 1 1 d . . . C40 C 0.4813(4) 0.43769(13) -0.0537(3) 0.0222(9) Uani 1 1 d . . . H40 H 0.5338 0.4513 -0.0932 0.027 Uiso 1 1 calc R . . C41 C 0.4362(5) 0.39269(14) -0.0664(3) 0.0280(9) Uani 1 1 d . . . H41 H 0.4574 0.3759 -0.1144 0.034 Uiso 1 1 calc R . . C42 C 0.3612(5) 0.37279(14) -0.0095(3) 0.0278(9) Uani 1 1 d . . . H42 H 0.3316 0.3420 -0.0179 0.033 Uiso 1 1 calc R . . C43 C 0.3279(5) 0.39700(14) 0.0604(3) 0.0283(9) Uani 1 1 d . . . H43 H 0.2747 0.3831 0.0992 0.034 Uiso 1 1 calc R . . C44 C 0.3734(4) 0.44167(13) 0.0728(3) 0.0226(8) Uani 1 1 d . . . H44 H 0.3517 0.4583 0.1210 0.027 Uiso 1 1 calc R . . P5 P 0.71501(10) 0.78477(3) 0.46016(6) 0.0173(2) Uani 1 1 d . . . P6 P 0.44441(11) 0.74918(3) 0.66015(6) 0.0167(2) Uani 1 1 d . . . P7 P 0.55875(10) 0.78714(3) 0.81400(6) 0.0169(2) Uani 1 1 d . . . P8 P 1.00718(11) 0.78759(3) 0.99748(6) 0.01673(19) Uani 1 1 d . . . O3 O 0.5611(3) 0.74743(9) 0.59142(15) 0.0191(6) Uani 1 1 d . . . O4 O 0.7410(3) 0.80448(8) 0.84282(15) 0.0178(6) Uani 1 1 d . . . N3 N 0.5593(3) 0.73584(10) 0.76370(19) 0.0179(7) Uani 1 1 d . . . N4 N 0.4761(3) 0.80193(10) 0.70315(19) 0.0157(6) Uani 1 1 d . . . C45 C 0.8402(4) 0.77418(12) 0.3844(2) 0.0168(8) Uani 1 1 d . . . C46 C 0.9856(4) 0.75647(14) 0.4219(3) 0.0248(9) Uani 1 1 d . . . H46 H 1.0143 0.7490 0.4841 0.030 Uiso 1 1 calc R . . C47 C 1.0897(4) 0.74946(14) 0.3708(3) 0.0272(9) Uani 1 1 d . . . H47 H 1.1886 0.7376 0.3984 0.033 Uiso 1 1 calc R . . C48 C 1.0505(5) 0.75962(13) 0.2806(3) 0.0239(9) Uani 1 1 d . . . H48 H 1.1218 0.7550 0.2454 0.029 Uiso 1 1 calc R . . C49 C 0.9059(5) 0.77671(13) 0.2416(3) 0.0236(9) Uani 1 1 d . . . H49 H 0.8778 0.7836 0.1791 0.028 Uiso 1 1 calc R . . C50 C 0.8004(4) 0.78409(13) 0.2923(2) 0.0215(8) Uani 1 1 d . . . H50 H 0.7015 0.7959 0.2644 0.026 Uiso 1 1 calc R . . C51 C 0.5771(4) 0.82458(13) 0.3908(2) 0.0176(8) Uani 1 1 d . . . C52 C 0.6171(4) 0.87012(14) 0.4006(3) 0.0253(9) Uani 1 1 d . . . H52 H 0.7073 0.8790 0.4446 0.030 Uiso 1 1 calc R . . C53 C 0.5265(5) 0.90245(14) 0.3470(3) 0.0282(10) Uani 1 1 d . . . H53 H 0.5549 0.9333 0.3542 0.034 Uiso 1 1 calc R . . C54 C 0.3956(5) 0.88995(14) 0.2833(3) 0.0281(10) Uani 1 1 d . . . H54 H 0.3341 0.9122 0.2463 0.034 Uiso 1 1 calc R . . C55 C 0.3534(5) 0.84530(15) 0.2731(3) 0.0299(10) Uani 1 1 d . . . H55 H 0.2628 0.8368 0.2289 0.036 Uiso 1 1 calc R . . C56 C 0.4428(4) 0.81248(13) 0.3272(2) 0.0231(9) Uani 1 1 d . . . H56 H 0.4121 0.7818 0.3207 0.028 Uiso 1 1 calc R . . C57 C 0.6036(4) 0.73206(12) 0.4484(2) 0.0165(8) Uani 1 1 d . . . C58 C 0.5841(4) 0.70291(13) 0.3742(3) 0.0233(9) Uani 1 1 d . . . H58 H 0.6292 0.7106 0.3267 0.028 Uiso 1 1 calc R . . C59 C 0.5008(5) 0.66314(14) 0.3684(3) 0.0271(9) Uani 1 1 d . . . H59 H 0.4871 0.6443 0.3170 0.033 Uiso 1 1 calc R . . C60 C 0.4384(4) 0.65141(13) 0.4379(2) 0.0199(8) Uani 1 1 d . . . H60 H 0.3819 0.6241 0.4343 0.024 Uiso 1 1 calc R . . C61 C 0.4566(4) 0.67882(12) 0.5134(2) 0.0175(8) Uani 1 1 d . . . H61 H 0.4149 0.6701 0.5617 0.021 Uiso 1 1 calc R . . C62 C 0.5366(4) 0.71917(12) 0.5172(2) 0.0148(7) Uani 1 1 d . . . C63 C 0.5886(4) 0.69047(13) 0.8058(2) 0.0192(8) Uani 1 1 d . . . C64 C 0.4381(5) 0.66511(15) 0.7952(3) 0.0331(10) Uani 1 1 d . . . H64A H 0.3693 0.6828 0.8220 0.050 Uiso 1 1 calc R . . H64B H 0.4586 0.6359 0.8257 0.050 Uiso 1 1 calc R . . H64C H 0.3895 0.6603 0.7310 0.050 Uiso 1 1 calc R . . C65 C 0.6919(5) 0.66468(15) 0.7596(3) 0.0329(10) Uani 1 1 d . . . H65A H 0.6409 0.6617 0.6953 0.049 Uiso 1 1 calc R . . H65B H 0.7127 0.6347 0.7867 0.049 Uiso 1 1 calc R . . H65C H 0.7890 0.6810 0.7670 0.049 Uiso 1 1 calc R . . C66 C 0.6665(6) 0.69599(16) 0.9060(3) 0.0405(12) Uani 1 1 d . . . H66A H 0.7668 0.7105 0.9134 0.061 Uiso 1 1 calc R . . H66B H 0.6807 0.6663 0.9350 0.061 Uiso 1 1 calc R . . H66C H 0.6021 0.7147 0.9340 0.061 Uiso 1 1 calc R . . C67 C 0.3970(4) 0.84488(13) 0.6679(3) 0.0210(8) Uani 1 1 d . . . C68 C 0.2795(5) 0.83554(15) 0.5804(3) 0.0336(10) Uani 1 1 d . . . H68A H 0.3306 0.8225 0.5371 0.050 Uiso 1 1 calc R . . H68B H 0.2288 0.8638 0.5561 0.050 Uiso 1 1 calc R . . H68C H 0.2028 0.8143 0.5910 0.050 Uiso 1 1 calc R . . C69 C 0.5195(5) 0.87734(14) 0.6529(4) 0.0436(12) Uani 1 1 d . . . H69A H 0.5981 0.8817 0.7097 0.065 Uiso 1 1 calc R . . H69B H 0.4718 0.9064 0.6317 0.065 Uiso 1 1 calc R . . H69C H 0.5671 0.8648 0.6077 0.065 Uiso 1 1 calc R . . C70 C 0.3199(4) 0.86454(13) 0.7372(3) 0.0312(10) Uani 1 1 d . . . H70A H 0.2375 0.8443 0.7439 0.047 Uiso 1 1 calc R . . H70B H 0.2766 0.8942 0.7167 0.047 Uiso 1 1 calc R . . H70C H 0.3961 0.8677 0.7953 0.047 Uiso 1 1 calc R . . C71 C 0.8631(4) 0.78821(13) 0.8120(2) 0.0163(7) Uani 1 1 d . . . C72 C 0.8536(4) 0.78483(14) 0.7216(2) 0.0179(8) Uani 1 1 d . . . H72 H 0.7640 0.7948 0.6784 0.022 Uiso 1 1 calc R . . C73 C 0.9767(4) 0.76666(13) 0.6939(2) 0.0199(8) Uani 1 1 d . . . H73 H 0.9707 0.7638 0.6314 0.024 Uiso 1 1 calc R . . C74 C 1.1067(4) 0.75288(13) 0.7569(2) 0.0199(8) Uani 1 1 d . . . H74 H 1.1888 0.7395 0.7378 0.024 Uiso 1 1 calc R . . C75 C 1.1187(4) 0.75846(13) 0.8480(2) 0.0191(8) Uani 1 1 d . . . H75 H 1.2103 0.7496 0.8908 0.023 Uiso 1 1 calc R . . C76 C 0.9981(4) 0.77698(11) 0.8780(2) 0.0147(7) Uani 1 1 d . . . C77 C 1.0492(4) 0.84848(12) 1.0049(2) 0.0161(8) Uani 1 1 d . . . C78 C 1.0260(4) 0.87172(13) 1.0786(2) 0.0202(8) Uani 1 1 d . . . H78 H 0.9884 0.8560 1.1223 0.024 Uiso 1 1 calc R . . C79 C 1.0568(4) 0.91757(14) 1.0897(3) 0.0250(9) Uani 1 1 d . . . H79 H 1.0405 0.9330 1.1406 0.030 Uiso 1 1 calc R . . C80 C 1.1117(4) 0.94071(14) 1.0257(3) 0.0266(9) Uani 1 1 d . . . H80 H 1.1325 0.9721 1.0324 0.032 Uiso 1 1 calc R . . C81 C 1.1360(4) 0.91759(14) 0.9519(3) 0.0256(9) Uani 1 1 d . . . H81 H 1.1747 0.9332 0.9085 0.031 Uiso 1 1 calc R . . C82 C 1.1045(4) 0.87245(13) 0.9412(2) 0.0219(8) Uani 1 1 d . . . H82 H 1.1204 0.8572 0.8899 0.026 Uiso 1 1 calc R . . C83 C 1.1973(4) 0.76349(13) 1.0501(2) 0.0208(8) Uani 1 1 d . . . C84 C 1.2028(5) 0.71981(13) 1.0817(3) 0.0259(9) Uani 1 1 d . . . H84 H 1.1095 0.7043 1.0789 0.031 Uiso 1 1 calc R . . C85 C 1.3412(5) 0.69808(15) 1.1173(3) 0.0334(10) Uani 1 1 d . . . H85 H 1.3425 0.6680 1.1386 0.040 Uiso 1 1 calc R . . C86 C 1.4777(5) 0.72046(15) 1.1216(3) 0.0302(10) Uani 1 1 d . . . H86 H 1.5730 0.7056 1.1453 0.036 Uiso 1 1 calc R . . C87 C 1.4755(5) 0.76403(14) 1.0918(3) 0.0289(9) Uani 1 1 d . . . H87 H 1.5697 0.7794 1.0958 0.035 Uiso 1 1 calc R . . C88 C 1.3365(4) 0.78616(14) 1.0557(2) 0.0241(8) Uani 1 1 d . . . H88 H 1.3359 0.8164 1.0350 0.029 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 P1 0.0157(5) 0.0170(5) 0.0156(5) -0.0001(4) 0.0052(3) -0.0031(4) P2 0.0135(4) 0.0167(5) 0.0156(5) -0.0001(4) 0.0052(4) -0.0009(4) P3 0.0134(4) 0.0190(5) 0.0155(5) -0.0021(4) 0.0047(3) -0.0005(4) P4 0.0181(5) 0.0192(5) 0.0149(5) 0.0006(4) 0.0029(4) -0.0021(4) O1 0.0133(13) 0.0190(14) 0.0196(13) -0.0015(10) 0.0044(10) 0.0006(11) O2 0.0188(13) 0.0209(14) 0.0164(13) -0.0050(11) 0.0059(10) -0.0071(12) N1 0.0176(16) 0.0150(16) 0.0165(16) -0.0009(12) 0.0043(13) -0.0003(13) N2 0.0155(16) 0.0141(15) 0.0158(16) 0.0014(12) 0.0029(12) 0.0015(12) C1 0.0130(17) 0.0125(19) 0.020(2) -0.0029(14) 0.0052(14) -0.0034(14) C2 0.0173(18) 0.021(2) 0.0182(19) -0.0001(16) 0.0031(14) -0.0046(17) C3 0.029(2) 0.022(2) 0.020(2) 0.0005(15) 0.0070(16) -0.0062(18) C4 0.026(2) 0.025(2) 0.032(2) -0.0057(17) 0.0184(18) -0.0075(18) C5 0.018(2) 0.030(2) 0.033(2) -0.0012(19) 0.0062(17) 0.0044(19) C6 0.022(2) 0.024(2) 0.021(2) 0.0029(16) 0.0046(16) -0.0047(17) C7 0.0155(19) 0.021(2) 0.0135(18) 0.0012(14) 0.0067(14) 0.0011(16) C8 0.022(2) 0.017(2) 0.027(2) -0.0010(16) 0.0073(16) -0.0022(16) C9 0.019(2) 0.028(2) 0.034(2) 0.0071(18) 0.0038(17) 0.0043(18) C10 0.026(2) 0.020(2) 0.037(2) 0.0062(17) 0.0130(18) 0.0058(17) C11 0.030(2) 0.021(2) 0.029(2) -0.0025(17) 0.0179(18) -0.0028(18) C12 0.020(2) 0.024(2) 0.023(2) -0.0027(16) 0.0083(16) -0.0052(17) C13 0.0144(18) 0.0131(19) 0.020(2) 0.0007(14) 0.0058(15) 0.0015(14) C14 0.022(2) 0.025(2) 0.020(2) -0.0001(16) 0.0105(16) -0.0068(17) C15 0.027(2) 0.025(2) 0.021(2) -0.0093(16) 0.0104(17) -0.0035(17) C16 0.019(2) 0.0140(19) 0.029(2) -0.0027(15) 0.0050(16) -0.0032(16) C17 0.0168(19) 0.019(2) 0.022(2) 0.0012(15) 0.0063(15) 0.0013(16) C18 0.0145(18) 0.018(2) 0.0130(18) -0.0023(14) 0.0007(14) 0.0019(15) C19 0.019(2) 0.021(2) 0.023(2) 0.0045(16) 0.0050(16) 0.0027(16) C20 0.025(2) 0.035(3) 0.045(3) 0.014(2) 0.0167(19) 0.019(2) C21 0.023(2) 0.016(2) 0.043(3) 0.0063(17) 0.0114(18) -0.0013(17) C22 0.054(3) 0.024(2) 0.027(2) 0.0097(19) 0.001(2) -0.005(2) C23 0.0122(18) 0.019(2) 0.0167(19) -0.0037(15) 0.0018(14) -0.0010(15) C24 0.021(2) 0.022(2) 0.037(2) 0.0068(18) -0.0018(17) -0.0011(17) C25 0.030(2) 0.021(2) 0.036(2) 0.0073(17) 0.0119(19) 0.0036(17) C26 0.031(2) 0.018(2) 0.025(2) 0.0011(16) 0.0017(18) 0.0064(17) C27 0.0147(18) 0.0152(19) 0.0210(19) -0.0030(16) 0.0069(14) -0.0065(16) C28 0.0120(17) 0.021(2) 0.0203(19) 0.0009(16) 0.0021(13) -0.0050(16) C29 0.0179(19) 0.026(2) 0.0165(19) -0.0016(15) 0.0064(15) -0.0056(16) C30 0.0147(19) 0.029(2) 0.024(2) -0.0009(17) 0.0096(15) 0.0021(17) C31 0.0133(18) 0.024(2) 0.0160(19) 0.0027(15) 0.0021(14) 0.0022(16) C32 0.0151(18) 0.018(2) 0.0121(18) 0.0021(13) 0.0024(13) -0.0022(15) C33 0.024(2) 0.023(2) 0.0141(19) 0.0036(15) 0.0023(15) 0.0014(17) C34 0.029(2) 0.026(2) 0.030(2) 0.0065(18) 0.0113(18) -0.0029(18) C35 0.046(3) 0.023(2) 0.035(2) 0.0086(19) 0.015(2) 0.010(2) C36 0.039(3) 0.034(3) 0.027(2) 0.0074(19) -0.0007(19) 0.015(2) C37 0.022(2) 0.046(3) 0.037(3) 0.001(2) -0.0102(18) -0.001(2) C38 0.023(2) 0.026(2) 0.030(2) -0.0028(17) -0.0088(17) -0.0044(17) C39 0.0148(19) 0.016(2) 0.020(2) 0.0030(15) 0.0004(15) 0.0042(15) C40 0.0152(19) 0.026(2) 0.024(2) 0.0064(16) 0.0025(16) -0.0019(17) C41 0.022(2) 0.025(2) 0.034(2) -0.0044(18) 0.0019(18) 0.0068(18) C42 0.023(2) 0.015(2) 0.039(3) 0.0020(17) -0.0037(18) 0.0033(17) C43 0.025(2) 0.027(2) 0.030(2) 0.0096(18) 0.0021(17) -0.0035(18) C44 0.022(2) 0.021(2) 0.023(2) 0.0010(16) 0.0037(16) 0.0039(16) P5 0.0162(5) 0.0206(5) 0.0154(5) -0.0012(4) 0.0049(4) -0.0042(4) P6 0.0139(5) 0.0195(5) 0.0171(5) -0.0016(4) 0.0047(4) -0.0015(4) P7 0.0134(4) 0.0210(5) 0.0166(5) -0.0020(4) 0.0045(4) 0.0008(4) P8 0.0169(5) 0.0188(5) 0.0145(4) -0.0004(4) 0.0041(3) -0.0011(4) O3 0.0185(14) 0.0236(15) 0.0163(13) -0.0037(11) 0.0067(10) -0.0045(11) O4 0.0136(13) 0.0222(14) 0.0174(13) -0.0046(10) 0.0039(10) 0.0020(11) N3 0.0199(17) 0.0200(18) 0.0151(16) -0.0008(12) 0.0069(13) -0.0013(13) N4 0.0130(15) 0.0138(16) 0.0186(16) 0.0018(12) 0.0010(12) 0.0029(12) C45 0.0196(19) 0.014(2) 0.0182(19) -0.0020(13) 0.0066(15) -0.0047(15) C46 0.021(2) 0.032(2) 0.020(2) -0.0007(17) 0.0031(16) 0.0025(18) C47 0.017(2) 0.031(2) 0.033(2) -0.0002(18) 0.0043(17) 0.0035(18) C48 0.023(2) 0.019(2) 0.033(2) -0.0080(17) 0.0132(18) -0.0057(17) C49 0.030(2) 0.025(2) 0.019(2) -0.0021(15) 0.0119(17) -0.0032(18) C50 0.021(2) 0.021(2) 0.022(2) 0.0014(17) 0.0025(15) -0.0016(18) C51 0.019(2) 0.018(2) 0.0183(19) 0.0006(15) 0.0094(15) -0.0021(16) C52 0.019(2) 0.027(2) 0.029(2) -0.0055(17) 0.0047(16) 0.0019(18) C53 0.028(2) 0.017(2) 0.040(3) -0.0027(17) 0.0095(19) 0.0000(18) C54 0.026(2) 0.031(2) 0.029(2) 0.0061(18) 0.0125(18) 0.0088(19) C55 0.023(2) 0.031(2) 0.032(2) -0.0012(18) -0.0006(18) -0.0015(19) C56 0.021(2) 0.020(2) 0.028(2) -0.0014(16) 0.0052(16) 0.0006(17) C57 0.0150(19) 0.019(2) 0.0147(19) -0.0014(14) 0.0021(14) -0.0017(15) C58 0.026(2) 0.025(2) 0.023(2) -0.0050(16) 0.0135(17) -0.0043(18) C59 0.030(2) 0.027(2) 0.025(2) -0.0103(17) 0.0082(18) -0.0050(19) C60 0.021(2) 0.0155(19) 0.024(2) 0.0000(16) 0.0078(16) -0.0036(16) C61 0.0165(19) 0.021(2) 0.0149(19) 0.0018(14) 0.0045(15) -0.0021(16) C62 0.0098(17) 0.018(2) 0.0142(19) -0.0017(14) -0.0005(14) 0.0042(14) C63 0.020(2) 0.015(2) 0.023(2) 0.0060(15) 0.0057(16) 0.0019(16) C64 0.026(2) 0.028(3) 0.045(3) 0.011(2) 0.009(2) -0.0012(19) C65 0.036(3) 0.032(3) 0.034(2) 0.0072(19) 0.015(2) 0.011(2) C66 0.060(3) 0.029(3) 0.025(2) 0.0051(19) -0.002(2) -0.006(2) C67 0.0166(19) 0.0147(19) 0.032(2) 0.0056(16) 0.0068(16) 0.0026(15) C68 0.034(3) 0.031(2) 0.031(2) 0.0030(18) -0.0009(19) 0.0092(19) C69 0.030(2) 0.027(2) 0.076(4) 0.015(2) 0.015(2) 0.002(2) C70 0.027(2) 0.024(2) 0.041(3) -0.0003(18) 0.0046(19) 0.0106(18) C71 0.0125(17) 0.0141(18) 0.0225(19) 0.0001(15) 0.0049(14) 0.0008(16) C72 0.0116(17) 0.021(2) 0.0188(19) -0.0010(16) -0.0003(14) 0.0001(16) C73 0.021(2) 0.027(2) 0.0130(19) -0.0014(15) 0.0058(15) -0.0069(17) C74 0.017(2) 0.027(2) 0.019(2) -0.0025(16) 0.0096(15) 0.0006(17) C75 0.0134(18) 0.023(2) 0.019(2) 0.0006(15) 0.0005(15) -0.0034(16) C76 0.0179(18) 0.0118(18) 0.0149(18) -0.0039(13) 0.0049(14) -0.0030(14) C77 0.0127(18) 0.0152(19) 0.0188(19) 0.0002(14) 0.0012(14) 0.0017(15) C78 0.0166(19) 0.022(2) 0.019(2) -0.0005(15) -0.0002(15) 0.0016(16) C79 0.018(2) 0.029(2) 0.025(2) -0.0059(17) -0.0010(16) 0.0008(17) C80 0.022(2) 0.019(2) 0.036(2) -0.0020(17) 0.0007(18) -0.0005(17) C81 0.024(2) 0.025(2) 0.025(2) 0.0084(17) 0.0021(17) -0.0027(17) C82 0.021(2) 0.024(2) 0.018(2) 0.0016(16) -0.0003(15) -0.0028(17) C83 0.021(2) 0.027(2) 0.0136(18) -0.0026(15) 0.0033(15) 0.0049(17) C84 0.028(2) 0.025(2) 0.024(2) 0.0039(17) 0.0061(17) 0.0007(17) C85 0.035(3) 0.031(2) 0.033(2) 0.0144(19) 0.007(2) 0.009(2) C86 0.026(2) 0.037(3) 0.025(2) 0.0051(18) 0.0023(17) 0.0125(19) C87 0.022(2) 0.033(2) 0.028(2) 0.0014(18) -0.0010(17) -0.0001(18) C88 0.022(2) 0.019(2) 0.027(2) 0.0003(17) -0.0015(16) -0.0022(17) _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 P1 C7 1.835(4) . ? P1 C1 1.845(3) . ? P1 C13 1.850(4) . ? P2 O2 1.666(2) . ? P2 N2 1.697(3) . ? P2 N1 1.710(3) . ? P3 O1 1.670(3) . ? P3 N1 1.709(3) . ? P3 N2 1.716(3) . ? P4 C39 1.828(4) . ? P4 C32 1.837(3) . ? P4 C33 1.842(4) . ? O1 C27 1.393(4) . ? O2 C18 1.379(4) . ? N1 C19 1.483(5) . ? N2 C23 1.493(5) . ? C1 C2 1.382(5) . ? C1 C6 1.409(5) . ? C2 C3 1.379(5) . ? C2 H2 0.9500 . ? C3 C4 1.375(5) . ? C3 H3 0.9500 . ? C4 C5 1.378(5) . ? C4 H4 0.9500 . ? C5 C6 1.386(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.381(5) . ? C7 C8 1.395(5) . ? C8 C9 1.386(5) . ? C8 H8 0.9500 . ? C9 C10 1.390(6) . ? C9 H9 0.9500 . ? C10 C11 1.391(6) . ? C10 H10 0.9500 . ? C11 C12 1.386(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.384(5) . ? C13 C18 1.399(5) . ? C14 C15 1.391(5) . ? C14 H14 0.9500 . ? C15 C16 1.388(5) . ? C15 H15 0.9500 . ? C16 C17 1.379(5) . ? C16 H16 0.9500 . ? C17 C18 1.397(5) . ? C17 H17 0.9500 . ? C19 C21 1.518(5) . ? C19 C22 1.518(5) . ? C19 C20 1.540(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.512(5) . ? C23 C26 1.518(5) . ? C23 C24 1.524(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.378(5) . ? C27 C32 1.399(5) . ? C28 C29 1.394(5) . ? C28 H28 0.9500 . ? C29 C30 1.382(5) . ? C29 H29 0.9500 . ? C30 C31 1.383(5) . ? C30 H30 0.9500 . ? C31 C32 1.399(5) . ? C31 H31 0.9500 . ? C33 C38 1.387(5) . ? C33 C34 1.400(5) . ? C34 C35 1.370(6) . ? C34 H34 0.9500 . ? C35 C36 1.370(6) . ? C35 H35 0.9500 . ? C36 C37 1.385(6) . ? C36 H36 0.9500 . ? C37 C38 1.385(6) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.389(5) . ? C39 C44 1.401(5) . ? C40 C41 1.394(6) . ? C40 H40 0.9500 . ? C41 C42 1.369(6) . ? C41 H41 0.9500 . ? C42 C43 1.387(6) . ? C42 H42 0.9500 . ? C43 C44 1.385(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? P5 C51 1.841(4) . ? P5 C57 1.841(4) . ? P5 C45 1.845(4) . ? P6 O3 1.672(3) . ? P6 N4 1.693(3) . ? P6 N3 1.705(3) . ? P7 O4 1.667(3) . ? P7 N3 1.707(3) . ? P7 N4 1.730(3) . ? P8 C83 1.839(4) . ? P8 C77 1.843(4) . ? P8 C76 1.844(3) . ? O3 C62 1.386(4) . ? O4 C71 1.392(4) . ? N3 C63 1.487(5) . ? N4 C67 1.491(5) . ? C45 C46 1.390(5) . ? C45 C50 1.397(5) . ? C46 C47 1.385(5) . ? C46 H46 0.9500 . ? C47 C48 1.373(5) . ? C47 H47 0.9500 . ? C48 C49 1.382(6) . ? C48 H48 0.9500 . ? C49 C50 1.393(5) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C56 1.391(5) . ? C51 C52 1.396(5) . ? C52 C53 1.385(6) . ? C52 H52 0.9500 . ? C53 C54 1.374(6) . ? C53 H53 0.9500 . ? C54 C55 1.375(6) . ? C54 H54 0.9500 . ? C55 C56 1.394(6) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C62 1.399(5) . ? C57 C58 1.405(5) . ? C58 C59 1.389(5) . ? C58 H58 0.9500 . ? C59 C60 1.373(5) . ? C59 H59 0.9500 . ? C60 C61 1.391(5) . ? C60 H60 0.9500 . ? C61 C62 1.390(5) . ? C61 H61 0.9500 . ? C63 C65 1.516(5) . ? C63 C64 1.522(5) . ? C63 C66 1.527(5) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.506(5) . ? C67 C69 1.526(5) . ? C67 C70 1.529(5) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.373(5) . ? C71 C76 1.406(5) . ? C72 C73 1.395(5) . ? C72 H72 0.9500 . ? C73 C74 1.374(5) . ? C73 H73 0.9500 . ? C74 C75 1.387(5) . ? C74 H74 0.9500 . ? C75 C76 1.397(5) . ? C75 H75 0.9500 . ? C77 C78 1.387(5) . ? C77 C82 1.401(5) . ? C78 C79 1.390(5) . ? C78 H78 0.9500 . ? C79 C80 1.390(6) . ? C79 H79 0.9500 . ? C80 C81 1.389(6) . ? C80 H80 0.9500 . ? C81 C82 1.369(6) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.380(5) . ? C83 C88 1.405(5) . ? C84 C85 1.384(5) . ? C84 H84 0.9500 . ? C85 C86 1.383(6) . ? C85 H85 0.9500 . ? C86 C87 1.369(6) . ? C86 H86 0.9500 . ? C87 C88 1.396(5) . ? C87 H87 0.9500 . ? C88 H88 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 C7 P1 C1 100.88(16) . . ? C7 P1 C13 102.76(16) . . ? C1 P1 C13 101.71(16) . . ? O2 P2 N2 102.08(14) . . ? O2 P2 N1 105.14(14) . . ? N2 P2 N1 81.18(14) . . ? O2 P2 P3 115.34(9) . . ? O1 P3 N1 106.16(14) . . ? O1 P3 N2 108.41(13) . . ? N1 P3 N2 80.69(14) . . ? O1 P3 P2 120.18(9) . . ? C39 P4 C32 99.90(16) . . ? C39 P4 C33 101.59(17) . . ? C32 P4 C33 99.23(16) . . ? C27 O1 P3 127.8(2) . . ? C18 O2 P2 123.1(2) . . ? C19 N1 P3 129.8(2) . . ? C19 N1 P2 128.4(2) . . ? P3 N1 P2 97.89(15) . . ? C23 N2 P2 128.4(2) . . ? C23 N2 P3 129.2(2) . . ? P2 N2 P3 98.10(15) . . ? C2 C1 C6 118.0(3) . . ? C2 C1 P1 125.1(3) . . ? C6 C1 P1 116.9(3) . . ? C3 C2 C1 121.1(4) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.9(4) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.0(4) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.5(3) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C12 C7 C8 118.2(4) . . ? C12 C7 P1 116.9(3) . . ? C8 C7 P1 124.8(3) . . ? C9 C8 C7 121.2(4) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.7(4) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 119.5(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 119.9(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C7 C12 C11 121.4(4) . . ? C7 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C18 118.2(3) . . ? C14 C13 P1 123.0(3) . . ? C18 C13 P1 118.7(3) . . ? C13 C14 C15 121.7(3) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C16 C15 C14 119.3(3) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 120.1(4) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? O2 C18 C17 121.6(3) . . ? O2 C18 C13 118.0(3) . . ? C17 C18 C13 120.5(3) . . ? N1 C19 C21 110.7(3) . . ? N1 C19 C22 109.3(3) . . ? C21 C19 C22 109.6(3) . . ? N1 C19 C20 107.9(3) . . ? C21 C19 C20 109.5(3) . . ? C22 C19 C20 109.8(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N2 C23 C25 107.9(3) . . ? N2 C23 C26 108.4(3) . . ? C25 C23 C26 110.5(3) . . ? N2 C23 C24 110.1(3) . . ? C25 C23 C24 109.6(3) . . ? C26 C23 C24 110.3(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 O1 121.0(3) . . ? C28 C27 C32 122.0(3) . . ? O1 C27 C32 117.0(3) . . ? C27 C28 C29 119.3(3) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C30 C29 C28 120.0(3) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.0(3) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C32 121.4(3) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C31 C32 C27 117.2(3) . . ? C31 C32 P4 123.6(3) . . ? C27 C32 P4 119.0(3) . . ? C38 C33 C34 117.6(4) . . ? C38 C33 P4 125.3(3) . . ? C34 C33 P4 117.0(3) . . ? C35 C34 C33 121.4(4) . . ? C35 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? C36 C35 C34 120.6(4) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 119.1(4) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C38 C37 C36 120.6(4) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C33 120.6(4) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 119.7 . . ? C40 C39 C44 118.0(4) . . ? C40 C39 P4 118.7(3) . . ? C44 C39 P4 123.3(3) . . ? C39 C40 C41 120.9(4) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C42 C41 C40 119.8(4) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 120.8(4) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C44 C43 C42 119.1(4) . . ? C44 C43 H43 120.5 . . ? C42 C43 H43 120.5 . . ? C43 C44 C39 121.3(4) . . ? C43 C44 H44 119.3 . . ? C39 C44 H44 119.3 . . ? C51 P5 C57 102.63(17) . . ? C51 P5 C45 100.06(16) . . ? C57 P5 C45 101.54(16) . . ? O3 P6 N4 101.83(14) . . ? O3 P6 N3 104.65(14) . . ? N4 P6 N3 81.38(14) . . ? O4 P7 N3 106.10(14) . . ? O4 P7 N4 109.09(14) . . ? N3 P7 N4 80.28(14) . . ? C83 P8 C77 101.59(17) . . ? C83 P8 C76 99.65(16) . . ? C77 P8 C76 100.61(16) . . ? C62 O3 P6 123.1(2) . . ? C71 O4 P7 127.8(2) . . ? C63 N3 P6 127.8(3) . . ? C63 N3 P7 129.1(2) . . ? P6 N3 P7 98.25(16) . . ? C67 N4 P6 129.1(2) . . ? C67 N4 P7 128.2(2) . . ? P6 N4 P7 97.81(15) . . ? C46 C45 C50 117.8(3) . . ? C46 C45 P5 117.8(3) . . ? C50 C45 P5 124.3(3) . . ? C47 C46 C45 121.7(4) . . ? C47 C46 H46 119.2 . . ? C45 C46 H46 119.2 . . ? C48 C47 C46 120.3(4) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C47 C48 C49 119.0(4) . . ? C47 C48 H48 120.5 . . ? C49 C48 H48 120.5 . . ? C48 C49 C50 121.2(4) . . ? C48 C49 H49 119.4 . . ? C50 C49 H49 119.4 . . ? C49 C50 C45 120.0(4) . . ? C49 C50 H50 120.0 . . ? C45 C50 H50 120.0 . . ? C56 C51 C52 118.6(4) . . ? C56 C51 P5 125.1(3) . . ? C52 C51 P5 116.2(3) . . ? C53 C52 C51 120.6(4) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C54 C53 C52 120.1(4) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C55 120.2(4) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? C54 C55 C56 120.3(4) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C51 C56 C55 120.2(4) . . ? C51 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C62 C57 C58 117.2(3) . . ? C62 C57 P5 119.2(3) . . ? C58 C57 P5 123.5(3) . . ? C59 C58 C57 121.8(4) . . ? C59 C58 H58 119.1 . . ? C57 C58 H58 119.1 . . ? C60 C59 C58 119.2(4) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.4 . . ? C59 C60 C61 121.1(4) . . ? C59 C60 H60 119.4 . . ? C61 C60 H60 119.4 . . ? C62 C61 C60 119.1(3) . . ? C62 C61 H61 120.5 . . ? C60 C61 H61 120.5 . . ? O3 C62 C61 121.7(3) . . ? O3 C62 C57 116.6(3) . . ? C61 C62 C57 121.6(3) . . ? N3 C63 C65 108.3(3) . . ? N3 C63 C64 110.3(3) . . ? C65 C63 C64 109.8(4) . . ? N3 C63 C66 109.0(3) . . ? C65 C63 C66 110.4(4) . . ? C64 C63 C66 109.0(3) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N4 C67 C68 109.1(3) . . ? N4 C67 C69 107.3(3) . . ? C68 C67 C69 110.5(4) . . ? N4 C67 C70 109.5(3) . . ? C68 C67 C70 110.5(3) . . ? C69 C67 C70 109.9(4) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C67 C70 H70A 109.5 . . ? C67 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C67 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 O4 121.4(3) . . ? C72 C71 C76 121.9(3) . . ? O4 C71 C76 116.7(3) . . ? C71 C72 C73 119.4(3) . . ? C71 C72 H72 120.3 . . ? C73 C72 H72 120.3 . . ? C74 C73 C72 120.0(3) . . ? C74 C73 H73 120.0 . . ? C72 C73 H73 120.0 . . ? C73 C74 C75 120.4(3) . . ? C73 C74 H74 119.8 . . ? C75 C74 H74 119.8 . . ? C74 C75 C76 121.0(3) . . ? C74 C75 H75 119.5 . . ? C76 C75 H75 119.5 . . ? C75 C76 C71 117.2(3) . . ? C75 C76 P8 123.8(3) . . ? C71 C76 P8 119.0(3) . . ? C78 C77 C82 118.3(4) . . ? C78 C77 P8 117.8(3) . . ? C82 C77 P8 124.0(3) . . ? C77 C78 C79 121.3(4) . . ? C77 C78 H78 119.4 . . ? C79 C78 H78 119.4 . . ? C78 C79 C80 119.5(4) . . ? C78 C79 H79 120.2 . . ? C80 C79 H79 120.2 . . ? C81 C80 C79 119.5(4) . . ? C81 C80 H80 120.2 . . ? C79 C80 H80 120.2 . . ? C82 C81 C80 120.6(4) . . ? C82 C81 H81 119.7 . . ? C80 C81 H81 119.7 . . ? C81 C82 C77 120.8(4) . . ? C81 C82 H82 119.6 . . ? C77 C82 H82 119.6 . . ? C84 C83 C88 118.5(4) . . ? C84 C83 P8 117.7(3) . . ? C88 C83 P8 123.8(3) . . ? C83 C84 C85 121.5(4) . . ? C83 C84 H84 119.2 . . ? C85 C84 H84 119.2 . . ? C86 C85 C84 119.6(4) . . ? C86 C85 H85 120.2 . . ? C84 C85 H85 120.2 . . ? C87 C86 C85 120.1(4) . . ? C87 C86 H86 120.0 . . ? C85 C86 H86 120.0 . . ? C86 C87 C88 120.7(4) . . ? C86 C87 H87 119.7 . . ? C88 C87 H87 119.7 . . ? C87 C88 C83 119.6(4) . . ? C87 C88 H88 120.2 . . ? C83 C88 H88 120.2 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.75 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.740 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.071 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 779799' #TrackingRef '- MSB-94.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tert-Butyl-[1,3-di-tert-butyl-4-(2-diphenylphosphanyl phenoxy)-[1,3,2,4]diazaphosphetidin-2-yl)amine ; _chemical_name_common ; tert-Butyl-(1,3-di-tert-butyl-4-(2-diphenylphosphanyl phenoxy)-(1,3,2,4)diazaphosphetidin-2-yl)amine ; _chemical_melting_point ? _chemical_formula_moiety 'C30 H42 N3 O P3' _chemical_formula_sum 'C30 H42 N3 O P3' _chemical_formula_weight 553.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall ' -P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0386(4) _cell_length_b 11.3565(4) _cell_length_c 16.0380(6) _cell_angle_alpha 74.097(1) _cell_angle_beta 87.839(1) _cell_angle_gamma 85.701(1) _cell_volume 1578.5(1) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9981 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 29.18 _exptl_crystal_description Column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9187 _exptl_absorpt_correction_T_max 0.9694 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 20 sec/frame. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27546 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 28.00 _reflns_number_total 7534 _reflns_number_gt 6102 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006a)' _computing_structure_solution 'Bruker XM (Bruker-AXS 2006)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2006)' _publ_section_references ; Bruker-AXS (2006). APEX2, Version 2.1-0, Madison, WI. Bruker-AXS (2006a). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2007). SADABS, Version 2007/2. University of G\"ottingen, Germany. ; _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. H-atoms attached to carbon were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. That attached to nitrogen was located in a difference map and refined with an isotropic displacement parameter ; _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^)+(0.0519P)^2^+0.3944P] 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 7534 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1093 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 P1 P 0.13760(4) 0.28215(4) 0.23734(3) 0.03571(11) Uani 1 1 d . . . P2 P 0.12822(4) 0.09039(3) 0.36972(2) 0.03071(10) Uani 1 1 d . . . P3 P 0.47047(4) -0.14586(3) 0.27986(3) 0.03486(10) Uani 1 1 d . . . O1 O 0.21632(12) -0.02937(9) 0.34099(6) 0.0363(2) Uani 1 1 d . . . N1 N 0.23231(18) 0.25316(15) 0.15396(9) 0.0483(4) Uani 1 1 d . . . N2 N 0.03130(13) 0.15828(11) 0.27967(8) 0.0338(3) Uani 1 1 d . . . N3 N 0.24206(13) 0.20386(11) 0.32638(8) 0.0334(3) Uani 1 1 d . . . C1 C 0.2601(2) 0.3346(2) 0.06691(12) 0.0603(5) Uani 1 1 d . . . C2 C 0.4231(3) 0.3182(3) 0.04394(18) 0.0968(9) Uani 1 1 d . . . H2A H 0.4832 0.3416 0.0857 0.145 Uiso 1 1 calc R . . H2B H 0.4429 0.3704 -0.0145 0.145 Uiso 1 1 calc R . . H2C H 0.4486 0.2322 0.0458 0.145 Uiso 1 1 calc R . . C3 C 0.2177(3) 0.4674(2) 0.06507(18) 0.0976(9) Uani 1 1 d . . . H3A H 0.1135 0.4754 0.0832 0.146 Uiso 1 1 calc R . . H3B H 0.2315 0.5201 0.0061 0.146 Uiso 1 1 calc R . . H3C H 0.2808 0.4923 0.1048 0.146 Uiso 1 1 calc R . . C4 C 0.1661(4) 0.2971(3) 0.00230(16) 0.1133(12) Uani 1 1 d . . . H4A H 0.1916 0.2108 0.0048 0.170 Uiso 1 1 calc R . . H4B H 0.1859 0.3485 -0.0564 0.170 Uiso 1 1 calc R . . H4C H 0.0607 0.3079 0.0171 0.170 Uiso 1 1 calc R . . C5 C -0.10316(17) 0.11967(15) 0.24827(11) 0.0406(4) Uani 1 1 d . . . C6 C -0.2010(2) 0.0637(2) 0.32661(14) 0.0587(5) Uani 1 1 d . . . H6A H -0.1473 -0.0081 0.3644 0.088 Uiso 1 1 calc R . . H6B H -0.2920 0.0387 0.3070 0.088 Uiso 1 1 calc R . . H6C H -0.2265 0.1246 0.3588 0.088 Uiso 1 1 calc R . . C7 C -0.0616(2) 0.02410(19) 0.19859(13) 0.0560(5) Uani 1 1 d . . . H7A H 0.0041 0.0592 0.1494 0.084 Uiso 1 1 calc R . . H7B H -0.1517 0.0002 0.1772 0.084 Uiso 1 1 calc R . . H7C H -0.0104 -0.0483 0.2373 0.084 Uiso 1 1 calc R . . C8 C -0.1850(2) 0.23170(19) 0.18887(16) 0.0649(6) Uani 1 1 d . . . H8A H -0.2141 0.2915 0.2214 0.097 Uiso 1 1 calc R . . H8B H -0.2738 0.2067 0.1669 0.097 Uiso 1 1 calc R . . H8C H -0.1197 0.2690 0.1401 0.097 Uiso 1 1 calc R . . C9 C 0.34377(17) 0.25485(16) 0.37505(11) 0.0415(4) Uani 1 1 d . . . C10 C 0.4294(2) 0.14795(19) 0.43717(13) 0.0553(5) Uani 1 1 d . . . H10A H 0.3602 0.0998 0.4791 0.083 Uiso 1 1 calc R . . H10B H 0.5018 0.1796 0.4681 0.083 Uiso 1 1 calc R . . H10C H 0.4814 0.0957 0.4044 0.083 Uiso 1 1 calc R . . C11 C 0.2577(3) 0.3345(2) 0.42592(16) 0.0687(6) Uani 1 1 d . . . H11A H 0.2026 0.4029 0.3856 0.103 Uiso 1 1 calc R . . H11B H 0.3273 0.3668 0.4581 0.103 Uiso 1 1 calc R . . H11C H 0.1881 0.2849 0.4666 0.103 Uiso 1 1 calc R . . C12 C 0.4509(2) 0.3307(2) 0.31103(15) 0.0698(6) Uani 1 1 d . . . H12A H 0.5039 0.2793 0.2780 0.105 Uiso 1 1 calc R . . H12B H 0.5224 0.3622 0.3425 0.105 Uiso 1 1 calc R . . H12C H 0.3957 0.3995 0.2712 0.105 Uiso 1 1 calc R . . C13 C 0.23990(16) -0.14451(13) 0.39718(9) 0.0302(3) Uani 1 1 d . . . C14 C 0.15091(17) -0.18854(15) 0.46994(10) 0.0379(3) Uani 1 1 d . . . H14 H 0.0707 -0.1379 0.4840 0.045 Uiso 1 1 calc R . . C15 C 0.18005(18) -0.30686(15) 0.52184(10) 0.0417(4) Uani 1 1 d . . . H15 H 0.1206 -0.3369 0.5723 0.050 Uiso 1 1 calc R . . C16 C 0.29495(19) -0.38150(15) 0.50084(11) 0.0425(4) Uani 1 1 d . . . H16 H 0.3141 -0.4627 0.5365 0.051 Uiso 1 1 calc R . . C17 C 0.38211(17) -0.33725(14) 0.42752(10) 0.0383(3) Uani 1 1 d . . . H17 H 0.4601 -0.3893 0.4129 0.046 Uiso 1 1 calc R . . C18 C 0.35751(15) -0.21792(13) 0.37493(9) 0.0306(3) Uani 1 1 d . . . C19 C 0.61589(18) -0.26772(14) 0.27938(11) 0.0434(4) Uani 1 1 d . . . C20 C 0.7421(2) -0.26951(18) 0.32678(15) 0.0577(5) Uani 1 1 d . . . H20 H 0.7469 -0.2119 0.3596 0.069 Uiso 1 1 calc R . . C21 C 0.8612(2) -0.3542(2) 0.32688(18) 0.0796(8) Uani 1 1 d . . . H21 H 0.9462 -0.3548 0.3601 0.095 Uiso 1 1 calc R . . C22 C 0.8561(3) -0.4372(2) 0.27898(18) 0.0907(10) Uani 1 1 d . . . H22 H 0.9379 -0.4946 0.2783 0.109 Uiso 1 1 calc R . . C23 C 0.7324(3) -0.4365(2) 0.23221(16) 0.0844(9) Uani 1 1 d . . . H23 H 0.7290 -0.4943 0.1994 0.101 Uiso 1 1 calc R . . C24 C 0.6115(3) -0.35284(17) 0.23179(13) 0.0607(5) Uani 1 1 d . . . H24 H 0.5264 -0.3539 0.1991 0.073 Uiso 1 1 calc R . . C25 C 0.35127(18) -0.15257(15) 0.19158(10) 0.0406(4) Uani 1 1 d . . . C26 C 0.2379(2) -0.23072(19) 0.19990(12) 0.0553(5) Uani 1 1 d . . . H26 H 0.2198 -0.2872 0.2545 0.066 Uiso 1 1 calc R . . C27 C 0.1504(3) -0.2283(2) 0.13020(14) 0.0725(6) Uani 1 1 d . . . H27 H 0.0733 -0.2828 0.1372 0.087 Uiso 1 1 calc R . . C28 C 0.1754(3) -0.1470(3) 0.05112(15) 0.0817(7) Uani 1 1 d . . . H28 H 0.1157 -0.1454 0.0033 0.098 Uiso 1 1 calc R . . C29 C 0.2853(3) -0.0687(3) 0.04111(14) 0.0811(7) Uani 1 1 d . . . H29 H 0.3023 -0.0126 -0.0138 0.097 Uiso 1 1 calc R . . C30 C 0.3732(2) -0.0704(2) 0.11090(12) 0.0594(5) Uani 1 1 d . . . H30 H 0.4490 -0.0146 0.1033 0.071 Uiso 1 1 calc R . . H1N H 0.271(2) 0.181(2) 0.1597(13) 0.059(6) Uiso 1 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 P1 0.0320(2) 0.0293(2) 0.0427(2) -0.00523(16) -0.00270(16) 0.00125(15) P2 0.02823(18) 0.0313(2) 0.03261(19) -0.00998(15) 0.00367(14) 0.00055(14) P3 0.0333(2) 0.0289(2) 0.0425(2) -0.01076(16) 0.00737(16) -0.00245(15) O1 0.0430(6) 0.0317(5) 0.0304(5) -0.0055(4) 0.0056(4) 0.0082(4) N1 0.0585(9) 0.0412(8) 0.0371(7) 0.0000(6) 0.0055(6) 0.0040(7) N2 0.0255(6) 0.0325(6) 0.0415(7) -0.0070(5) -0.0021(5) -0.0009(5) N3 0.0304(6) 0.0333(6) 0.0361(6) -0.0087(5) -0.0012(5) -0.0030(5) C1 0.0557(11) 0.0686(13) 0.0426(10) 0.0099(9) 0.0001(8) -0.0109(10) C2 0.0681(15) 0.115(2) 0.0795(17) 0.0168(15) 0.0242(13) -0.0056(15) C3 0.109(2) 0.0627(16) 0.0877(18) 0.0321(13) 0.0073(16) 0.0027(15) C4 0.122(2) 0.163(3) 0.0436(13) 0.0016(16) -0.0130(14) -0.043(2) C5 0.0297(7) 0.0413(9) 0.0528(9) -0.0161(7) -0.0060(7) -0.0009(6) C6 0.0384(9) 0.0753(14) 0.0691(13) -0.0274(11) 0.0060(9) -0.0222(9) C7 0.0543(11) 0.0616(12) 0.0612(12) -0.0312(10) -0.0113(9) -0.0008(9) C8 0.0421(10) 0.0564(12) 0.0914(16) -0.0111(11) -0.0273(10) 0.0054(9) C9 0.0338(8) 0.0456(9) 0.0481(9) -0.0164(8) -0.0048(7) -0.0058(7) C10 0.0456(10) 0.0638(12) 0.0561(11) -0.0142(9) -0.0161(8) -0.0007(9) C11 0.0673(13) 0.0702(14) 0.0846(15) -0.0479(13) -0.0145(11) 0.0021(11) C12 0.0514(11) 0.0810(16) 0.0724(14) -0.0045(12) -0.0072(10) -0.0340(11) C13 0.0327(7) 0.0293(7) 0.0285(7) -0.0085(6) -0.0020(5) 0.0010(6) C14 0.0374(8) 0.0383(8) 0.0353(8) -0.0080(6) 0.0056(6) 0.0036(6) C15 0.0444(9) 0.0403(9) 0.0359(8) -0.0041(7) 0.0083(7) -0.0029(7) C16 0.0473(9) 0.0308(8) 0.0439(9) -0.0016(7) 0.0021(7) -0.0002(7) C17 0.0377(8) 0.0299(8) 0.0456(9) -0.0092(7) 0.0023(7) 0.0023(6) C18 0.0307(7) 0.0305(7) 0.0324(7) -0.0115(6) 0.0007(5) -0.0026(6) C19 0.0428(9) 0.0312(8) 0.0512(9) -0.0058(7) 0.0196(7) -0.0005(6) C20 0.0411(9) 0.0449(10) 0.0774(13) -0.0029(9) 0.0106(9) 0.0021(8) C21 0.0464(11) 0.0628(14) 0.1015(18) 0.0172(13) 0.0210(12) 0.0139(10) C22 0.0895(18) 0.0532(13) 0.0916(18) 0.0254(13) 0.0574(16) 0.0353(13) C23 0.126(2) 0.0429(11) 0.0680(15) -0.0033(10) 0.0474(16) 0.0270(13) C24 0.0810(14) 0.0402(10) 0.0572(11) -0.0126(9) 0.0216(10) 0.0061(9) C25 0.0440(9) 0.0418(9) 0.0365(8) -0.0130(7) 0.0084(7) -0.0019(7) C26 0.0663(12) 0.0630(12) 0.0413(9) -0.0186(9) 0.0035(8) -0.0202(10) C27 0.0790(15) 0.0961(18) 0.0533(12) -0.0332(12) -0.0019(11) -0.0264(13) C28 0.0848(17) 0.122(2) 0.0447(12) -0.0309(13) -0.0065(11) -0.0108(16) C29 0.0905(18) 0.108(2) 0.0347(10) -0.0029(11) 0.0033(11) -0.0055(16) C30 0.0606(12) 0.0668(13) 0.0441(10) -0.0042(9) 0.0085(9) -0.0077(10) _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 P1 N1 1.6559(15) . ? P1 N2 1.7300(13) . ? P1 N3 1.7324(13) . ? P2 N2 1.6828(13) . ? P2 O1 1.6880(10) . ? P2 N3 1.6901(13) . ? P3 C25 1.8324(17) . ? P3 C18 1.8333(15) . ? P3 C19 1.8372(16) . ? O1 C13 1.3763(17) . ? N1 C1 1.473(2) . ? N1 H1N 0.85(2) . ? N2 C5 1.4731(19) . ? N3 C9 1.474(2) . ? C1 C2 1.515(3) . ? C1 C3 1.521(3) . ? C1 C4 1.529(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.524(2) . ? C5 C6 1.526(2) . ? C5 C7 1.531(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C12 1.516(3) . ? C9 C10 1.523(2) . ? C9 C11 1.530(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.389(2) . ? C13 C18 1.3978(19) . ? C14 C15 1.385(2) . ? C14 H14 0.9500 . ? C15 C16 1.382(2) . ? C15 H15 0.9500 . ? C16 C17 1.386(2) . ? C16 H16 0.9500 . ? C17 C18 1.393(2) . ? C17 H17 0.9500 . ? C19 C24 1.389(3) . ? C19 C20 1.390(3) . ? C20 C21 1.389(3) . ? C20 H20 0.9500 . ? C21 C22 1.373(4) . ? C21 H21 0.9500 . ? C22 C23 1.368(4) . ? C22 H22 0.9500 . ? C23 C24 1.393(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.384(2) . ? C25 C30 1.390(2) . ? C26 C27 1.387(3) . ? C26 H26 0.9500 . ? C27 C28 1.371(3) . ? C27 H27 0.9500 . ? C28 C29 1.358(4) . ? C28 H28 0.9500 . ? C29 C30 1.392(3) . ? C29 H29 0.9500 . ? C30 H30 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 N1 P1 N2 106.41(7) . . ? N1 P1 N3 103.99(7) . . ? N2 P1 N3 79.74(6) . . ? N2 P2 O1 100.81(6) . . ? N2 P2 N3 82.30(6) . . ? O1 P2 N3 101.80(6) . . ? C25 P3 C18 101.09(7) . . ? C25 P3 C19 102.49(8) . . ? C18 P3 C19 101.93(7) . . ? C13 O1 P2 123.60(9) . . ? C1 N1 P1 129.77(14) . . ? C1 N1 H1N 112.2(14) . . ? P1 N1 H1N 118.0(14) . . ? C5 N2 P2 129.07(11) . . ? C5 N2 P1 131.91(11) . . ? P2 N2 P1 99.02(6) . . ? C9 N3 P2 125.73(11) . . ? C9 N3 P1 127.71(11) . . ? P2 N3 P1 98.64(6) . . ? N1 C1 C2 108.49(17) . . ? N1 C1 C3 110.31(18) . . ? C2 C1 C3 110.6(2) . . ? N1 C1 C4 108.31(18) . . ? C2 C1 C4 109.6(2) . . ? C3 C1 C4 109.6(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C8 108.87(14) . . ? N2 C5 C6 108.24(14) . . ? C8 C5 C6 110.14(15) . . ? N2 C5 C7 110.27(13) . . ? C8 C5 C7 109.78(16) . . ? C6 C5 C7 109.52(15) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C12 108.34(14) . . ? N3 C9 C10 107.96(14) . . ? C12 C9 C10 109.57(15) . . ? N3 C9 C11 110.85(14) . . ? C12 C9 C11 110.14(17) . . ? C10 C9 C11 109.93(16) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C13 C14 123.16(13) . . ? O1 C13 C18 115.66(12) . . ? C14 C13 C18 121.15(13) . . ? C15 C14 C13 119.44(14) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C16 C15 C14 120.48(14) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 119.67(15) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 121.24(14) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C13 118.00(13) . . ? C17 C18 P3 125.51(11) . . ? C13 C18 P3 116.46(11) . . ? C24 C19 C20 118.42(17) . . ? C24 C19 P3 124.72(16) . . ? C20 C19 P3 116.77(14) . . ? C21 C20 C19 121.0(2) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 120.0(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 119.5(2) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 121.3(2) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C19 C24 C23 119.7(2) . . ? C19 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C30 117.52(17) . . ? C26 C25 P3 124.89(13) . . ? C30 C25 P3 117.56(14) . . ? C25 C26 C27 121.38(19) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C28 C27 C26 119.8(2) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 120.1(2) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.3(2) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C25 C30 C29 120.8(2) . . ? C25 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.235 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.048 #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 779800' #TrackingRef '- MSB-94.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tert-Butyl-[1,3-di-tert-butyl-4-(2-diphenythiophosphorylphenoxy)- 2,4-dithio-[1,3,2,4]diazadiphosphetidin-2-yl)amine ; _chemical_name_common ; tert-Butyl-(1,3-di-tert-butyl-4-(2- diphenythiophosphorylphenoxy)-2,4-dithio-(1,3,2,4)diazadiphosphetidin-2- yl)amine ; _chemical_melting_point ? _chemical_formula_moiety 'C30 H42 N3 O P3 S3' _chemical_formula_sum 'C30 H42 N3 O P3 S3' _chemical_formula_weight 649.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0885(9) _cell_length_b 14.8388(10) _cell_length_c 16.1937(11) _cell_angle_alpha 90.134(1) _cell_angle_beta 97.004(1) _cell_angle_gamma 90.529(1) _cell_volume 3360.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9453 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.28 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9167 _exptl_absorpt_correction_T_max 0.9440 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 29808 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15143 _reflns_number_gt 12957 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SMART (Bruker-AXS, 2000)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. ; _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. H-atoms attached to carbon were placed in calculated positions (C---H = 0.95 - 0.98 \%A) while those attached to nitrogen were placed in positions derived from a difference map. All were included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached atoms. ; _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^)+(0.0494P)^2^+0.8920P] 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 15143 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 P1 P 0.16367(3) 0.29963(3) 1.05969(3) 0.01563(9) Uani 1 1 d . . . P2 P 0.18277(3) 0.19432(3) 0.94300(3) 0.01719(9) Uani 1 1 d . . . P3 P 0.49325(3) 0.23712(3) 0.96643(2) 0.01454(9) Uani 1 1 d . . . S1 S 0.04586(3) 0.31815(3) 1.10628(3) 0.02335(10) Uani 1 1 d . . . S2 S 0.09096(3) 0.11354(3) 0.88399(3) 0.02989(11) Uani 1 1 d . . . S3 S 0.46835(3) 0.25177(3) 1.08205(2) 0.01835(9) Uani 1 1 d . . . O1 O 0.28561(8) 0.19742(7) 0.90827(7) 0.0173(2) Uani 1 1 d . . . N1 N 0.16003(9) 0.30262(9) 0.95408(8) 0.0166(3) Uani 1 1 d . . . N2 N 0.25484(9) 0.35885(9) 1.10121(8) 0.0171(3) Uani 1 1 d . . . H2N H 0.3094 0.3420 1.0900 0.020 Uiso 1 1 d R . . N3 N 0.19984(9) 0.19194(9) 1.04659(8) 0.0168(3) Uani 1 1 d . . . C1 C 0.11476(12) 0.36878(12) 0.89204(10) 0.0216(3) Uani 1 1 d . . . C2 C 0.15946(13) 0.35587(13) 0.81145(11) 0.0273(4) Uani 1 1 d . . . H2A H 0.2290 0.3638 0.8227 0.041 Uiso 1 1 calc R . . H2B H 0.1335 0.4005 0.7704 0.041 Uiso 1 1 calc R . . H2C H 0.1446 0.2951 0.7896 0.041 Uiso 1 1 calc R . . C3 C 0.13637(14) 0.46351(12) 0.92690(12) 0.0291(4) Uani 1 1 d . . . H3A H 0.1076 0.4707 0.9786 0.044 Uiso 1 1 calc R . . H3B H 0.1096 0.5081 0.8862 0.044 Uiso 1 1 calc R . . H3C H 0.2058 0.4724 0.9382 0.044 Uiso 1 1 calc R . . C4 C 0.00657(12) 0.35292(14) 0.87701(11) 0.0281(4) Uani 1 1 d . . . H4A H -0.0067 0.2914 0.8564 0.042 Uiso 1 1 calc R . . H4B H -0.0221 0.3960 0.8357 0.042 Uiso 1 1 calc R . . H4C H -0.0208 0.3612 0.9293 0.042 Uiso 1 1 calc R . . C5 C 0.26870(12) 0.42609(11) 1.17100(10) 0.0195(3) Uani 1 1 d . . . C6 C 0.36974(12) 0.46379(12) 1.17092(12) 0.0269(4) Uani 1 1 d . . . H6A H 0.4158 0.4145 1.1787 0.040 Uiso 1 1 calc R . . H6B H 0.3834 0.5076 1.2163 0.040 Uiso 1 1 calc R . . H6C H 0.3750 0.4935 1.1177 0.040 Uiso 1 1 calc R . . C7 C 0.19798(13) 0.50363(12) 1.15677(12) 0.0278(4) Uani 1 1 d . . . H7A H 0.2058 0.5334 1.1040 0.042 Uiso 1 1 calc R . . H7B H 0.2102 0.5472 1.2025 0.042 Uiso 1 1 calc R . . H7C H 0.1325 0.4800 1.1547 0.042 Uiso 1 1 calc R . . C8 C 0.25986(13) 0.38057(12) 1.25389(11) 0.0252(4) Uani 1 1 d . . . H8A H 0.1950 0.3559 1.2535 0.038 Uiso 1 1 calc R . . H8B H 0.2726 0.4248 1.2990 0.038 Uiso 1 1 calc R . . H8C H 0.3063 0.3317 1.2625 0.038 Uiso 1 1 calc R . . C9 C 0.20674(12) 0.11298(11) 1.10428(11) 0.0222(4) Uani 1 1 d . . . C10 C 0.27173(13) 0.04414(12) 1.07027(12) 0.0270(4) Uani 1 1 d . . . H10A H 0.2426 0.0232 1.0155 0.040 Uiso 1 1 calc R . . H10B H 0.2804 -0.0072 1.1083 0.040 Uiso 1 1 calc R . . H10C H 0.3340 0.0721 1.0651 0.040 Uiso 1 1 calc R . . C11 C 0.10755(14) 0.07143(13) 1.11019(13) 0.0334(4) Uani 1 1 d . . . H11A H 0.0668 0.1162 1.1327 0.050 Uiso 1 1 calc R . . H11B H 0.1140 0.0189 1.1470 0.050 Uiso 1 1 calc R . . H11C H 0.0785 0.0526 1.0547 0.050 Uiso 1 1 calc R . . C12 C 0.25183(14) 0.14538(12) 1.18963(11) 0.0280(4) Uani 1 1 d . . . H12A H 0.3137 0.1742 1.1846 0.042 Uiso 1 1 calc R . . H12B H 0.2613 0.0939 1.2274 0.042 Uiso 1 1 calc R . . H12C H 0.2095 0.1889 1.2118 0.042 Uiso 1 1 calc R . . C13 C 0.34329(11) 0.12644(11) 0.88881(10) 0.0165(3) Uani 1 1 d . . . C14 C 0.30749(12) 0.05208(11) 0.84310(10) 0.0206(3) Uani 1 1 d . . . H14 H 0.2417 0.0488 0.8216 0.025 Uiso 1 1 calc R . . C15 C 0.36851(13) -0.01780(11) 0.82884(10) 0.0225(4) Uani 1 1 d . . . H15 H 0.3439 -0.0693 0.7982 0.027 Uiso 1 1 calc R . . C16 C 0.46445(13) -0.01315(11) 0.85876(10) 0.0219(3) Uani 1 1 d . . . H16 H 0.5052 -0.0623 0.8510 0.026 Uiso 1 1 calc R . . C17 C 0.50082(12) 0.06414(11) 0.90033(10) 0.0198(3) Uani 1 1 d . . . H17 H 0.5673 0.0683 0.9190 0.024 Uiso 1 1 calc R . . C18 C 0.44156(11) 0.13565(10) 0.91509(9) 0.0156(3) Uani 1 1 d . . . C19 C 0.45080(11) 0.32927(10) 0.89922(10) 0.0163(3) Uani 1 1 d . . . C20 C 0.43951(11) 0.31998(11) 0.81264(10) 0.0201(3) Uani 1 1 d . . . H20 H 0.4509 0.2635 0.7880 0.024 Uiso 1 1 calc R . . C21 C 0.41161(12) 0.39329(12) 0.76264(11) 0.0235(4) Uani 1 1 d . . . H21 H 0.4048 0.3873 0.7038 0.028 Uiso 1 1 calc R . . C22 C 0.39373(12) 0.47517(12) 0.79858(12) 0.0250(4) Uani 1 1 d . . . H22 H 0.3742 0.5251 0.7642 0.030 Uiso 1 1 calc R . . C23 C 0.40405(12) 0.48476(11) 0.88415(12) 0.0242(4) Uani 1 1 d . . . H23 H 0.3915 0.5411 0.9084 0.029 Uiso 1 1 calc R . . C24 C 0.43277(11) 0.41199(11) 0.93476(11) 0.0194(3) Uani 1 1 d . . . H24 H 0.4401 0.4187 0.9936 0.023 Uiso 1 1 calc R . . C25 C 0.62103(11) 0.22877(11) 0.95866(10) 0.0179(3) Uani 1 1 d . . . C26 C 0.65948(13) 0.24824(13) 0.88564(12) 0.0298(4) Uani 1 1 d . . . H26 H 0.6194 0.2696 0.8384 0.036 Uiso 1 1 calc R . . C27 C 0.75672(14) 0.23637(15) 0.88165(13) 0.0361(5) Uani 1 1 d . . . H27 H 0.7826 0.2494 0.8315 0.043 Uiso 1 1 calc R . . C28 C 0.81578(13) 0.20582(13) 0.94981(13) 0.0309(4) Uani 1 1 d . . . H28 H 0.8821 0.1977 0.9467 0.037 Uiso 1 1 calc R . . C29 C 0.77797(13) 0.18713(13) 1.02248(12) 0.0292(4) Uani 1 1 d . . . H29 H 0.8184 0.1660 1.0696 0.035 Uiso 1 1 calc R . . C30 C 0.68112(12) 0.19903(12) 1.02736(11) 0.0242(4) Uani 1 1 d . . . H30 H 0.6559 0.1867 1.0780 0.029 Uiso 1 1 calc R . . S4 S 0.77371(3) 0.48116(3) 0.38714(3) 0.02283(10) Uani 1 1 d . . . S5 S 0.63260(3) 0.37617(3) 0.62937(3) 0.02307(10) Uani 1 1 d . . . S6 S 0.72280(3) 0.07805(3) 0.39042(2) 0.01944(9) Uani 1 1 d . . . P4 P 0.76750(3) 0.35832(3) 0.42522(2) 0.01507(9) Uani 1 1 d . . . P5 P 0.69609(3) 0.30820(3) 0.55129(2) 0.01504(9) Uani 1 1 d . . . P6 P 0.74468(3) 0.02476(3) 0.50115(3) 0.01506(9) Uani 1 1 d . . . O2 O 0.71003(8) 0.20266(7) 0.57392(7) 0.0170(2) Uani 1 1 d . . . N4 N 0.80301(9) 0.33806(9) 0.52784(8) 0.0151(3) Uani 1 1 d . . . N5 N 0.81400(10) 0.28495(9) 0.36776(8) 0.0180(3) Uani 1 1 d . . . H5N H 0.8000 0.2322 0.3798 0.022 Uiso 1 1 d R . . N6 N 0.66154(9) 0.31606(9) 0.44949(8) 0.0154(3) Uani 1 1 d . . . C31 C 0.88961(12) 0.36888(11) 0.58411(10) 0.0200(3) Uani 1 1 d . . . C32 C 0.90120(13) 0.30559(13) 0.65873(11) 0.0273(4) Uani 1 1 d . . . H32A H 0.8471 0.3129 0.6909 0.041 Uiso 1 1 calc R . . H32B H 0.9609 0.3201 0.6940 0.041 Uiso 1 1 calc R . . H32C H 0.9030 0.2431 0.6392 0.041 Uiso 1 1 calc R . . C33 C 0.87707(14) 0.46590(13) 0.61214(12) 0.0304(4) Uani 1 1 d . . . H33A H 0.8730 0.5059 0.5638 0.046 Uiso 1 1 calc R . . H33B H 0.9319 0.4838 0.6521 0.046 Uiso 1 1 calc R . . H33C H 0.8183 0.4703 0.6385 0.046 Uiso 1 1 calc R . . C34 C 0.97639(12) 0.36243(13) 0.53660(11) 0.0240(4) Uani 1 1 d . . . H34A H 0.9820 0.3006 0.5166 0.036 Uiso 1 1 calc R . . H34B H 1.0343 0.3789 0.5736 0.036 Uiso 1 1 calc R . . H34C H 0.9687 0.4037 0.4891 0.036 Uiso 1 1 calc R . . C35 C 0.86753(12) 0.29243(11) 0.29352(10) 0.0216(3) Uani 1 1 d . . . C36 C 0.89883(15) 0.19716(13) 0.27450(12) 0.0338(5) Uani 1 1 d . . . H36A H 0.9394 0.1734 0.3229 0.051 Uiso 1 1 calc R . . H36B H 0.9349 0.1986 0.2265 0.051 Uiso 1 1 calc R . . H36C H 0.8423 0.1583 0.2619 0.051 Uiso 1 1 calc R . . C37 C 0.80307(14) 0.32810(14) 0.21854(11) 0.0305(4) Uani 1 1 d . . . H37A H 0.7467 0.2888 0.2070 0.046 Uiso 1 1 calc R . . H37B H 0.8383 0.3292 0.1700 0.046 Uiso 1 1 calc R . . H37C H 0.7827 0.3893 0.2304 0.046 Uiso 1 1 calc R . . C38 C 0.95545(14) 0.35275(15) 0.31240(12) 0.0352(5) Uani 1 1 d . . . H38A H 0.9357 0.4132 0.3272 0.053 Uiso 1 1 calc R . . H38B H 0.9895 0.3563 0.2632 0.053 Uiso 1 1 calc R . . H38C H 0.9978 0.3276 0.3590 0.053 Uiso 1 1 calc R . . C39 C 0.56352(11) 0.31539(11) 0.40254(10) 0.0188(3) Uani 1 1 d . . . C40 C 0.51825(13) 0.40851(12) 0.40624(12) 0.0269(4) Uani 1 1 d . . . H40A H 0.5124 0.4240 0.4642 0.040 Uiso 1 1 calc R . . H40B H 0.4547 0.4076 0.3740 0.040 Uiso 1 1 calc R . . H40C H 0.5587 0.4535 0.3828 0.040 Uiso 1 1 calc R . . C41 C 0.57088(12) 0.28770(12) 0.31286(10) 0.0228(4) Uani 1 1 d . . . H41A H 0.6124 0.3305 0.2879 0.034 Uiso 1 1 calc R . . H41B H 0.5071 0.2876 0.2811 0.034 Uiso 1 1 calc R . . H41C H 0.5979 0.2271 0.3119 0.034 Uiso 1 1 calc R . . C42 C 0.50405(12) 0.24495(12) 0.44255(11) 0.0240(4) Uani 1 1 d . . . H42A H 0.5354 0.1863 0.4422 0.036 Uiso 1 1 calc R . . H42B H 0.4402 0.2407 0.4111 0.036 Uiso 1 1 calc R . . H42C H 0.4984 0.2627 0.5001 0.036 Uiso 1 1 calc R . . C43 C 0.64715(11) 0.13881(10) 0.59979(10) 0.0156(3) Uani 1 1 d . . . C44 C 0.58230(12) 0.15786(11) 0.65502(10) 0.0218(3) Uani 1 1 d . . . H44 H 0.5787 0.2170 0.6770 0.026 Uiso 1 1 calc R . . C45 C 0.52248(12) 0.08974(12) 0.67798(11) 0.0238(4) Uani 1 1 d . . . H45 H 0.4773 0.1027 0.7153 0.029 Uiso 1 1 calc R . . C46 C 0.52803(12) 0.00335(12) 0.64704(11) 0.0241(4) Uani 1 1 d . . . H46 H 0.4865 -0.0427 0.6626 0.029 Uiso 1 1 calc R . . C47 C 0.59424(12) -0.01571(11) 0.59328(11) 0.0209(3) Uani 1 1 d . . . H47 H 0.5981 -0.0752 0.5722 0.025 Uiso 1 1 calc R . . C48 C 0.65570(11) 0.05140(11) 0.56948(10) 0.0160(3) Uani 1 1 d . . . C49 C 0.85809(11) 0.05608(11) 0.56001(10) 0.0179(3) Uani 1 1 d . . . C50 C 0.87402(13) 0.04104(13) 0.64513(11) 0.0284(4) Uani 1 1 d . . . H50 H 0.8237 0.0189 0.6738 0.034 Uiso 1 1 calc R . . C51 C 0.96408(14) 0.05855(15) 0.68851(13) 0.0372(5) Uani 1 1 d . . . H51 H 0.9757 0.0468 0.7465 0.045 Uiso 1 1 calc R . . C52 C 1.03665(13) 0.09318(13) 0.64691(12) 0.0304(4) Uani 1 1 d . . . H52 H 1.0981 0.1048 0.6764 0.037 Uiso 1 1 calc R . . C53 C 1.01986(12) 0.11073(11) 0.56295(11) 0.0230(4) Uani 1 1 d . . . H53 H 1.0692 0.1362 0.5350 0.028 Uiso 1 1 calc R . . C54 C 0.93082(11) 0.09129(11) 0.51892(11) 0.0190(3) Uani 1 1 d . . . H54 H 0.9199 0.1021 0.4608 0.023 Uiso 1 1 calc R . . C55 C 0.74624(11) -0.09823(11) 0.49487(11) 0.0203(3) Uani 1 1 d . . . C56 C 0.72088(13) -0.13956(12) 0.41803(13) 0.0288(4) Uani 1 1 d . . . H56 H 0.6998 -0.1042 0.3706 0.035 Uiso 1 1 calc R . . C57 C 0.72636(15) -0.23278(13) 0.41075(15) 0.0403(5) Uani 1 1 d . . . H57 H 0.7098 -0.2607 0.3580 0.048 Uiso 1 1 calc R . . C58 C 0.75547(15) -0.28490(13) 0.47916(16) 0.0413(5) Uani 1 1 d . . . H58 H 0.7584 -0.3485 0.4738 0.050 Uiso 1 1 calc R . . C59 C 0.78035(15) -0.24448(13) 0.55535(14) 0.0356(5) Uani 1 1 d . . . H59 H 0.8007 -0.2804 0.6026 0.043 Uiso 1 1 calc R . . C60 C 0.77594(13) -0.15145(12) 0.56379(12) 0.0272(4) Uani 1 1 d . . . H60 H 0.7932 -0.1241 0.6167 0.033 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 P1 0.01286(18) 0.0189(2) 0.0157(2) -0.00036(15) 0.00373(15) 0.00051(15) P2 0.01313(19) 0.0212(2) 0.0175(2) -0.00351(16) 0.00287(15) -0.00288(16) P3 0.01459(19) 0.01435(19) 0.01493(19) 0.00027(15) 0.00283(15) 0.00040(15) S1 0.01630(19) 0.0317(2) 0.0236(2) -0.00109(17) 0.00855(16) 0.00162(17) S2 0.0200(2) 0.0377(3) 0.0318(3) -0.0140(2) 0.00353(18) -0.01131(19) S3 0.02022(19) 0.0198(2) 0.01560(19) -0.00046(15) 0.00444(15) 0.00223(15) O1 0.0144(5) 0.0187(6) 0.0195(6) -0.0041(4) 0.0048(4) -0.0011(4) N1 0.0145(6) 0.0207(7) 0.0144(6) -0.0005(5) 0.0009(5) 0.0017(5) N2 0.0124(6) 0.0200(7) 0.0194(7) -0.0046(5) 0.0044(5) 0.0010(5) N3 0.0172(6) 0.0171(7) 0.0167(7) -0.0009(5) 0.0040(5) -0.0008(5) C1 0.0187(8) 0.0278(9) 0.0184(8) 0.0046(7) 0.0025(6) 0.0053(7) C2 0.0230(9) 0.0387(11) 0.0205(9) 0.0059(7) 0.0038(7) 0.0039(8) C3 0.0306(10) 0.0278(10) 0.0290(10) 0.0057(8) 0.0028(8) 0.0058(8) C4 0.0158(8) 0.0445(11) 0.0237(9) 0.0036(8) 0.0009(7) 0.0067(8) C5 0.0201(8) 0.0183(8) 0.0203(8) -0.0051(6) 0.0030(6) 0.0017(6) C6 0.0221(9) 0.0280(9) 0.0311(10) -0.0116(8) 0.0052(7) -0.0049(7) C7 0.0298(10) 0.0232(9) 0.0301(10) -0.0064(7) 0.0016(8) 0.0072(7) C8 0.0289(9) 0.0270(9) 0.0198(9) -0.0033(7) 0.0028(7) 0.0030(7) C9 0.0258(9) 0.0177(8) 0.0243(9) 0.0027(7) 0.0082(7) -0.0008(7) C10 0.0342(10) 0.0184(9) 0.0302(10) 0.0036(7) 0.0112(8) 0.0025(7) C11 0.0316(10) 0.0290(10) 0.0426(12) 0.0054(8) 0.0163(9) -0.0070(8) C12 0.0382(11) 0.0249(9) 0.0220(9) 0.0075(7) 0.0073(8) 0.0020(8) C13 0.0186(8) 0.0175(8) 0.0142(7) 0.0009(6) 0.0053(6) 0.0008(6) C14 0.0217(8) 0.0222(8) 0.0181(8) -0.0029(6) 0.0033(6) -0.0028(7) C15 0.0331(9) 0.0165(8) 0.0185(8) -0.0029(6) 0.0061(7) -0.0035(7) C16 0.0302(9) 0.0151(8) 0.0212(8) -0.0001(6) 0.0055(7) 0.0051(7) C17 0.0210(8) 0.0194(8) 0.0191(8) 0.0016(6) 0.0035(6) 0.0018(6) C18 0.0204(8) 0.0142(7) 0.0128(7) 0.0011(6) 0.0040(6) -0.0017(6) C19 0.0145(7) 0.0154(8) 0.0192(8) 0.0030(6) 0.0029(6) -0.0003(6) C20 0.0189(8) 0.0208(8) 0.0207(8) 0.0017(6) 0.0029(6) -0.0014(6) C21 0.0208(8) 0.0270(9) 0.0222(9) 0.0059(7) 0.0012(7) -0.0041(7) C22 0.0195(8) 0.0207(9) 0.0339(10) 0.0111(7) -0.0010(7) -0.0015(7) C23 0.0208(8) 0.0162(8) 0.0350(10) 0.0017(7) 0.0018(7) -0.0003(7) C24 0.0164(8) 0.0187(8) 0.0232(8) -0.0011(6) 0.0028(6) -0.0022(6) C25 0.0144(7) 0.0163(8) 0.0235(8) -0.0013(6) 0.0042(6) -0.0011(6) C26 0.0225(9) 0.0396(11) 0.0287(10) 0.0091(8) 0.0083(7) 0.0048(8) C27 0.0245(10) 0.0464(12) 0.0407(12) 0.0110(9) 0.0172(9) 0.0041(9) C28 0.0172(8) 0.0289(10) 0.0477(12) -0.0039(9) 0.0081(8) 0.0001(7) C29 0.0196(9) 0.0342(10) 0.0323(10) -0.0045(8) -0.0025(7) 0.0049(7) C30 0.0200(8) 0.0302(10) 0.0225(9) -0.0002(7) 0.0030(7) 0.0025(7) S4 0.0291(2) 0.01458(19) 0.0251(2) 0.00263(16) 0.00463(17) -0.00396(16) S5 0.0258(2) 0.0195(2) 0.0262(2) -0.00752(16) 0.01293(17) -0.00234(17) S6 0.0212(2) 0.0196(2) 0.0174(2) 0.00030(15) 0.00174(15) -0.00287(16) P4 0.01644(19) 0.01369(19) 0.0154(2) -0.00017(15) 0.00356(15) -0.00280(15) P5 0.01566(19) 0.01398(19) 0.0162(2) -0.00260(15) 0.00506(15) -0.00272(15) P6 0.01344(19) 0.01433(19) 0.0176(2) -0.00049(15) 0.00280(15) -0.00225(15) O2 0.0179(5) 0.0144(5) 0.0198(6) -0.0003(4) 0.0071(4) -0.0032(4) N4 0.0152(6) 0.0168(6) 0.0138(6) -0.0015(5) 0.0041(5) -0.0042(5) N5 0.0236(7) 0.0141(6) 0.0177(7) -0.0002(5) 0.0088(6) -0.0032(5) N6 0.0139(6) 0.0163(7) 0.0163(7) -0.0003(5) 0.0028(5) -0.0020(5) C31 0.0180(8) 0.0244(9) 0.0176(8) -0.0046(6) 0.0027(6) -0.0082(7) C32 0.0253(9) 0.0384(11) 0.0174(8) 0.0001(7) -0.0003(7) -0.0082(8) C33 0.0319(10) 0.0283(10) 0.0320(10) -0.0145(8) 0.0092(8) -0.0133(8) C34 0.0174(8) 0.0316(10) 0.0229(9) -0.0027(7) 0.0026(7) -0.0059(7) C35 0.0260(9) 0.0232(9) 0.0175(8) -0.0021(6) 0.0106(7) -0.0063(7) C36 0.0453(12) 0.0298(10) 0.0312(10) -0.0009(8) 0.0241(9) 0.0029(9) C37 0.0367(11) 0.0377(11) 0.0181(9) -0.0001(7) 0.0066(8) -0.0027(8) C38 0.0286(10) 0.0517(13) 0.0279(10) -0.0109(9) 0.0152(8) -0.0166(9) C39 0.0160(8) 0.0162(8) 0.0234(8) 0.0008(6) -0.0008(6) -0.0002(6) C40 0.0232(9) 0.0210(9) 0.0360(10) -0.0011(7) 0.0008(8) 0.0048(7) C41 0.0219(8) 0.0236(9) 0.0217(9) 0.0010(7) -0.0027(7) -0.0002(7) C42 0.0179(8) 0.0236(9) 0.0301(10) 0.0020(7) 0.0014(7) -0.0042(7) C43 0.0146(7) 0.0165(8) 0.0155(8) 0.0026(6) 0.0019(6) -0.0040(6) C44 0.0261(9) 0.0203(8) 0.0204(8) -0.0006(6) 0.0088(7) -0.0019(7) C45 0.0217(8) 0.0278(9) 0.0238(9) 0.0010(7) 0.0108(7) -0.0024(7) C46 0.0201(8) 0.0225(9) 0.0306(10) 0.0038(7) 0.0073(7) -0.0059(7) C47 0.0191(8) 0.0170(8) 0.0269(9) -0.0008(7) 0.0042(7) -0.0048(6) C48 0.0131(7) 0.0193(8) 0.0157(8) 0.0015(6) 0.0020(6) -0.0012(6) C49 0.0158(7) 0.0161(8) 0.0217(8) 0.0008(6) 0.0013(6) -0.0013(6) C50 0.0230(9) 0.0376(11) 0.0237(9) 0.0078(8) -0.0002(7) -0.0105(8) C51 0.0297(10) 0.0532(13) 0.0259(10) 0.0118(9) -0.0069(8) -0.0129(9) C52 0.0190(9) 0.0340(10) 0.0355(11) 0.0038(8) -0.0074(8) -0.0062(7) C53 0.0154(8) 0.0208(9) 0.0335(10) -0.0009(7) 0.0057(7) -0.0024(6) C54 0.0169(8) 0.0176(8) 0.0230(8) -0.0017(6) 0.0046(6) 0.0004(6) C55 0.0153(8) 0.0162(8) 0.0306(9) -0.0008(7) 0.0072(7) -0.0013(6) C56 0.0239(9) 0.0221(9) 0.0388(11) -0.0066(8) -0.0024(8) -0.0021(7) C57 0.0363(11) 0.0240(10) 0.0588(14) -0.0161(10) -0.0007(10) -0.0037(8) C58 0.0361(11) 0.0165(9) 0.0736(16) -0.0015(10) 0.0162(11) -0.0008(8) C59 0.0374(11) 0.0220(9) 0.0510(13) 0.0132(9) 0.0189(10) 0.0046(8) C60 0.0295(10) 0.0214(9) 0.0331(10) 0.0039(7) 0.0137(8) 0.0007(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 P1 N2 1.6247(14) . ? P1 N3 1.7025(14) . ? P1 N1 1.7055(13) . ? P1 S1 1.9267(6) . ? P2 O1 1.6172(11) . ? P2 N1 1.6553(14) . ? P2 N3 1.6658(14) . ? P2 S2 1.9203(6) . ? P3 C19 1.8099(16) . ? P3 C18 1.8208(16) . ? P3 C25 1.8252(16) . ? P3 S3 1.9584(6) . ? O1 C13 1.3948(18) . ? N1 C1 1.497(2) . ? N2 C5 1.499(2) . ? N2 H2N 0.8501 . ? N3 C9 1.497(2) . ? C1 C3 1.528(3) . ? C1 C2 1.529(2) . ? C1 C4 1.530(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.522(2) . ? C5 C6 1.525(2) . ? C5 C7 1.528(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C12 1.524(2) . ? C9 C10 1.524(2) . ? C9 C11 1.536(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.384(2) . ? C13 C18 1.403(2) . ? C14 C15 1.390(2) . ? C14 H14 0.9500 . ? C15 C16 1.380(2) . ? C15 H15 0.9500 . ? C16 C17 1.390(2) . ? C16 H16 0.9500 . ? C17 C18 1.394(2) . ? C17 H17 0.9500 . ? C19 C24 1.393(2) . ? C19 C20 1.398(2) . ? C20 C21 1.388(2) . ? C20 H20 0.9500 . ? C21 C22 1.384(3) . ? C21 H21 0.9500 . ? C22 C23 1.382(3) . ? C22 H22 0.9500 . ? C23 C24 1.390(2) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.389(2) . ? C25 C26 1.389(2) . ? C26 C27 1.392(3) . ? C26 H26 0.9500 . ? C27 C28 1.379(3) . ? C27 H27 0.9500 . ? C28 C29 1.377(3) . ? C28 H28 0.9500 . ? C29 C30 1.389(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? S4 P4 1.9303(6) . ? S5 P5 1.9242(6) . ? S6 P6 1.9525(6) . ? P4 N5 1.6241(14) . ? P4 N6 1.7038(13) . ? P4 N4 1.7042(13) . ? P5 O2 1.6175(11) . ? P5 N4 1.6547(13) . ? P5 N6 1.6656(13) . ? P6 C49 1.8139(16) . ? P6 C48 1.8159(16) . ? P6 C55 1.8280(17) . ? O2 C43 1.3909(18) . ? N4 C31 1.498(2) . ? N5 C35 1.499(2) . ? N5 H5N 0.8342 . ? N6 C39 1.493(2) . ? C31 C34 1.526(2) . ? C31 C32 1.526(2) . ? C31 C33 1.527(2) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C38 1.521(2) . ? C35 C37 1.524(3) . ? C35 C36 1.527(2) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C41 1.524(2) . ? C39 C42 1.528(2) . ? C39 C40 1.531(2) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.385(2) . ? C43 C48 1.397(2) . ? C44 C45 1.390(2) . ? C44 H44 0.9500 . ? C45 C46 1.382(2) . ? C45 H45 0.9500 . ? C46 C47 1.382(2) . ? C46 H46 0.9500 . ? C47 C48 1.399(2) . ? C47 H47 0.9500 . ? C49 C54 1.387(2) . ? C49 C50 1.388(2) . ? C50 C51 1.395(2) . ? C50 H50 0.9500 . ? C51 C52 1.387(3) . ? C51 H51 0.9500 . ? C52 C53 1.377(3) . ? C52 H52 0.9500 . ? C53 C54 1.393(2) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.391(2) . ? C55 C60 1.393(2) . ? C56 C57 1.392(3) . ? C56 H56 0.9500 . ? C57 C58 1.376(3) . ? C57 H57 0.9500 . ? C58 C59 1.376(3) . ? C58 H58 0.9500 . ? C59 C60 1.389(3) . ? C59 H59 0.9500 . ? C60 H60 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 N2 P1 N3 108.62(7) . . ? N2 P1 N1 108.98(7) . . ? N3 P1 N1 82.81(7) . . ? N2 P1 S1 115.69(5) . . ? N3 P1 S1 118.35(5) . . ? N1 P1 S1 117.80(5) . . ? O1 P2 N1 102.16(6) . . ? O1 P2 N3 108.98(6) . . ? N1 P2 N3 85.48(7) . . ? O1 P2 S2 114.68(5) . . ? N1 P2 S2 121.75(5) . . ? N3 P2 S2 119.44(5) . . ? C19 P3 C18 105.41(7) . . ? C19 P3 C25 105.86(7) . . ? C18 P3 C25 104.37(7) . . ? C19 P3 S3 113.99(6) . . ? C18 P3 S3 114.77(5) . . ? C25 P3 S3 111.57(6) . . ? C13 O1 P2 129.34(10) . . ? C1 N1 P2 130.00(11) . . ? C1 N1 P1 130.57(11) . . ? P2 N1 P1 95.64(7) . . ? C5 N2 P1 133.50(11) . . ? C5 N2 H2N 108.8 . . ? P1 N2 H2N 116.2 . . ? C9 N3 P2 129.68(11) . . ? C9 N3 P1 131.18(11) . . ? P2 N3 P1 95.36(7) . . ? N1 C1 C3 108.03(14) . . ? N1 C1 C2 107.62(13) . . ? C3 C1 C2 110.35(15) . . ? N1 C1 C4 110.25(14) . . ? C3 C1 C4 109.93(15) . . ? C2 C1 C4 110.60(14) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C8 110.65(13) . . ? N2 C5 C6 105.81(13) . . ? C8 C5 C6 109.69(14) . . ? N2 C5 C7 111.52(14) . . ? C8 C5 C7 110.42(14) . . ? C6 C5 C7 108.62(15) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C12 108.14(13) . . ? N3 C9 C10 107.47(13) . . ? C12 C9 C10 109.53(15) . . ? N3 C9 C11 110.93(14) . . ? C12 C9 C11 110.30(15) . . ? C10 C9 C11 110.38(15) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 O1 122.61(14) . . ? C14 C13 C18 120.89(15) . . ? O1 C13 C18 116.45(13) . . ? C13 C14 C15 119.48(16) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.71(15) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 119.35(15) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C18 121.24(16) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C13 118.05(14) . . ? C17 C18 P3 119.58(12) . . ? C13 C18 P3 122.37(12) . . ? C24 C19 C20 119.62(15) . . ? C24 C19 P3 119.03(12) . . ? C20 C19 P3 121.31(12) . . ? C21 C20 C19 119.96(16) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 119.97(16) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.44(16) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.04(16) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 119.97(16) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C30 C25 C26 119.08(16) . . ? C30 C25 P3 118.67(13) . . ? C26 C25 P3 122.21(13) . . ? C25 C26 C27 119.97(18) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 120.64(18) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C29 C28 C27 119.50(17) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 120.42(18) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C25 C30 C29 120.37(17) . . ? C25 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? N5 P4 N6 108.40(7) . . ? N5 P4 N4 110.22(7) . . ? N6 P4 N4 82.59(6) . . ? N5 P4 S4 114.53(5) . . ? N6 P4 S4 119.30(5) . . ? N4 P4 S4 117.62(5) . . ? O2 P5 N4 102.44(6) . . ? O2 P5 N6 108.05(6) . . ? N4 P5 N6 85.27(7) . . ? O2 P5 S5 114.55(5) . . ? N4 P5 S5 121.53(5) . . ? N6 P5 S5 120.50(5) . . ? C49 P6 C48 104.72(7) . . ? C49 P6 C55 105.07(7) . . ? C48 P6 C55 105.67(7) . . ? C49 P6 S6 114.33(6) . . ? C48 P6 S6 115.17(5) . . ? C55 P6 S6 111.01(6) . . ? C43 O2 P5 131.27(10) . . ? C31 N4 P5 129.34(10) . . ? C31 N4 P4 131.28(10) . . ? P5 N4 P4 95.96(7) . . ? C35 N5 P4 133.57(11) . . ? C35 N5 H5N 114.3 . . ? P4 N5 H5N 111.8 . . ? C39 N6 P5 130.15(11) . . ? C39 N6 P4 131.56(11) . . ? P5 N6 P4 95.56(7) . . ? N4 C31 C34 108.42(13) . . ? N4 C31 C32 107.40(13) . . ? C34 C31 C32 109.98(15) . . ? N4 C31 C33 110.19(14) . . ? C34 C31 C33 110.11(14) . . ? C32 C31 C33 110.67(14) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N5 C35 C38 110.91(14) . . ? N5 C35 C37 110.80(14) . . ? C38 C35 C37 110.23(15) . . ? N5 C35 C36 106.35(13) . . ? C38 C35 C36 109.34(16) . . ? C37 C35 C36 109.10(15) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N6 C39 C41 108.56(13) . . ? N6 C39 C42 107.63(13) . . ? C41 C39 C42 109.05(14) . . ? N6 C39 C40 110.28(13) . . ? C41 C39 C40 110.93(14) . . ? C42 C39 C40 110.31(14) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 O2 123.24(14) . . ? C44 C43 C48 120.83(14) . . ? O2 C43 C48 115.87(13) . . ? C43 C44 C45 119.43(16) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C46 C45 C44 120.65(16) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 119.68(16) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? C46 C47 C48 120.89(16) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C43 C48 C47 118.46(14) . . ? C43 C48 P6 121.08(12) . . ? C47 C48 P6 120.46(12) . . ? C54 C49 C50 119.87(15) . . ? C54 C49 P6 119.63(13) . . ? C50 C49 P6 120.43(12) . . ? C49 C50 C51 119.85(17) . . ? C49 C50 H50 120.1 . . ? C51 C50 H50 120.1 . . ? C52 C51 C50 119.93(18) . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C53 C52 C51 120.12(17) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C52 C53 C54 120.19(16) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C49 C54 C53 119.98(16) . . ? C49 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C56 C55 C60 119.10(16) . . ? C56 C55 P6 118.81(14) . . ? C60 C55 P6 122.04(14) . . ? C55 C56 C57 119.92(19) . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C58 C57 C56 120.6(2) . . ? C58 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? C59 C58 C57 119.74(19) . . ? C59 C58 H58 120.1 . . ? C57 C58 H58 120.1 . . ? C58 C59 C60 120.50(19) . . ? C58 C59 H59 119.8 . . ? C60 C59 H59 119.7 . . ? C59 C60 C55 120.11(18) . . ? C59 C60 H60 119.9 . . ? C55 C60 H60 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 N2 P1 P2 O1 -5.54(8) . . . . ? N3 P1 P2 O1 -90.61(8) . . . . ? N1 P1 P2 O1 79.90(8) . . . . ? S1 P1 P2 O1 174.09(5) . . . . ? N2 P1 P2 N1 -85.44(9) . . . . ? N3 P1 P2 N1 -170.51(10) . . . . ? S1 P1 P2 N1 94.20(7) . . . . ? N2 P1 P2 N3 85.07(9) . . . . ? N1 P1 P2 N3 170.51(10) . . . . ? S1 P1 P2 N3 -95.30(7) . . . . ? N2 P1 P2 S2 177.89(6) . . . . ? N3 P1 P2 S2 92.82(8) . . . . ? N1 P1 P2 S2 -96.67(7) . . . . ? S1 P1 P2 S2 -2.47(5) . . . . ? N1 P2 O1 C13 178.25(13) . . . . ? N3 P2 O1 C13 88.89(13) . . . . ? S2 P2 O1 C13 -48.00(14) . . . . ? P1 P2 O1 C13 134.92(11) . . . . ? O1 P2 N1 C1 85.69(14) . . . . ? N3 P2 N1 C1 -165.84(14) . . . . ? S2 P2 N1 C1 -43.77(16) . . . . ? P1 P2 N1 C1 -159.38(17) . . . . ? O1 P2 N1 P1 -114.93(6) . . . . ? N3 P2 N1 P1 -6.47(7) . . . . ? S2 P2 N1 P1 115.60(5) . . . . ? N2 P1 N1 C1 -87.18(15) . . . . ? N3 P1 N1 C1 165.55(15) . . . . ? S1 P1 N1 C1 47.22(15) . . . . ? P2 P1 N1 C1 159.20(18) . . . . ? N2 P1 N1 P2 113.62(7) . . . . ? N3 P1 N1 P2 6.36(6) . . . . ? S1 P1 N1 P2 -111.98(5) . . . . ? N3 P1 N2 C5 -134.79(15) . . . . ? N1 P1 N2 C5 136.58(15) . . . . ? S1 P1 N2 C5 1.11(17) . . . . ? P2 P1 N2 C5 -179.22(13) . . . . ? O1 P2 N3 C9 -92.61(14) . . . . ? N1 P2 N3 C9 166.07(14) . . . . ? S2 P2 N3 C9 41.90(15) . . . . ? P1 P2 N3 C9 159.59(17) . . . . ? O1 P2 N3 P1 107.79(7) . . . . ? N1 P2 N3 P1 6.47(7) . . . . ? S2 P2 N3 P1 -117.69(5) . . . . ? N2 P1 N3 C9 86.92(15) . . . . ? N1 P1 N3 C9 -165.42(15) . . . . ? S1 P1 N3 C9 -47.64(16) . . . . ? P2 P1 N3 C9 -159.11(18) . . . . ? N2 P1 N3 P2 -113.97(7) . . . . ? N1 P1 N3 P2 -6.31(6) . . . . ? S1 P1 N3 P2 111.47(5) . . . . ? P2 N1 C1 C3 -164.18(12) . . . . ? P1 N1 C1 C3 43.30(19) . . . . ? P2 N1 C1 C2 -45.03(19) . . . . ? P1 N1 C1 C2 162.44(12) . . . . ? P2 N1 C1 C4 75.68(18) . . . . ? P1 N1 C1 C4 -76.85(18) . . . . ? P1 N2 C5 C8 67.43(19) . . . . ? P1 N2 C5 C6 -173.81(13) . . . . ? P1 N2 C5 C7 -55.9(2) . . . . ? P2 N3 C9 C12 163.12(12) . . . . ? P1 N3 C9 C12 -44.4(2) . . . . ? P2 N3 C9 C10 44.95(19) . . . . ? P1 N3 C9 C10 -162.52(12) . . . . ? P2 N3 C9 C11 -75.80(18) . . . . ? P1 N3 C9 C11 76.73(19) . . . . ? P2 O1 C13 C14 45.6(2) . . . . ? P2 O1 C13 C18 -137.02(12) . . . . ? O1 C13 C14 C15 -177.47(14) . . . . ? C18 C13 C14 C15 5.3(2) . . . . ? C13 C14 C15 C16 -0.9(2) . . . . ? C14 C15 C16 C17 -2.9(2) . . . . ? C15 C16 C17 C18 2.4(2) . . . . ? C16 C17 C18 C13 1.8(2) . . . . ? C16 C17 C18 P3 -177.77(12) . . . . ? C14 C13 C18 C17 -5.6(2) . . . . ? O1 C13 C18 C17 176.92(13) . . . . ? C14 C13 C18 P3 173.88(12) . . . . ? O1 C13 C18 P3 -3.55(19) . . . . ? C19 P3 C18 C17 127.37(13) . . . . ? C25 P3 C18 C17 16.07(15) . . . . ? S3 P3 C18 C17 -106.36(12) . . . . ? C19 P3 C18 C13 -52.15(14) . . . . ? C25 P3 C18 C13 -163.45(13) . . . . ? S3 P3 C18 C13 74.12(13) . . . . ? C18 P3 C19 C24 146.37(13) . . . . ? C25 P3 C19 C24 -103.39(13) . . . . ? S3 P3 C19 C24 19.62(14) . . . . ? C18 P3 C19 C20 -36.20(15) . . . . ? C25 P3 C19 C20 74.04(14) . . . . ? S3 P3 C19 C20 -162.96(11) . . . . ? C24 C19 C20 C21 0.8(2) . . . . ? P3 C19 C20 C21 -176.63(12) . . . . ? C19 C20 C21 C22 -0.9(2) . . . . ? C20 C21 C22 C23 0.4(3) . . . . ? C21 C22 C23 C24 0.2(3) . . . . ? C22 C23 C24 C19 -0.2(2) . . . . ? C20 C19 C24 C23 -0.2(2) . . . . ? P3 C19 C24 C23 177.25(12) . . . . ? C19 P3 C25 C30 148.86(13) . . . . ? C18 P3 C25 C30 -100.16(14) . . . . ? S3 P3 C25 C30 24.33(15) . . . . ? C19 P3 C25 C26 -33.35(17) . . . . ? C18 P3 C25 C26 77.63(16) . . . . ? S3 P3 C25 C26 -157.88(14) . . . . ? C30 C25 C26 C27 1.1(3) . . . . ? P3 C25 C26 C27 -176.70(16) . . . . ? C25 C26 C27 C28 -0.4(3) . . . . ? C26 C27 C28 C29 -0.1(3) . . . . ? C27 C28 C29 C30 -0.1(3) . . . . ? C26 C25 C30 C29 -1.3(3) . . . . ? P3 C25 C30 C29 176.52(14) . . . . ? C28 C29 C30 C25 0.9(3) . . . . ? N5 P4 P5 O2 5.80(8) . . . . ? N6 P4 P5 O2 89.97(8) . . . . ? N4 P4 P5 O2 -81.13(8) . . . . ? S4 P4 P5 O2 -174.09(5) . . . . ? N5 P4 P5 N4 86.94(9) . . . . ? N6 P4 P5 N4 171.10(10) . . . . ? S4 P4 P5 N4 -92.96(7) . . . . ? N5 P4 P5 N6 -84.16(9) . . . . ? N4 P4 P5 N6 -171.10(10) . . . . ? S4 P4 P5 N6 95.94(7) . . . . ? N5 P4 P5 S5 -177.77(6) . . . . ? N6 P4 P5 S5 -93.61(7) . . . . ? N4 P4 P5 S5 95.29(7) . . . . ? S4 P4 P5 S5 2.33(5) . . . . ? N4 P5 O2 C43 179.00(13) . . . . ? N6 P5 O2 C43 -91.96(14) . . . . ? S5 P5 O2 C43 45.41(14) . . . . ? P4 P5 O2 C43 -137.59(12) . . . . ? O2 P5 N4 C31 -85.88(14) . . . . ? N6 P5 N4 C31 166.66(14) . . . . ? S5 P5 N4 C31 43.51(15) . . . . ? P4 P5 N4 C31 160.60(17) . . . . ? O2 P5 N4 P4 113.52(6) . . . . ? N6 P5 N4 P4 6.06(6) . . . . ? S5 P5 N4 P4 -117.10(5) . . . . ? N5 P4 N4 C31 87.10(15) . . . . ? N6 P4 N4 C31 -165.96(15) . . . . ? S4 P4 N4 C31 -46.70(15) . . . . ? P5 P4 N4 C31 -160.01(18) . . . . ? N5 P4 N4 P5 -112.88(7) . . . . ? N6 P4 N4 P5 -5.95(6) . . . . ? S4 P4 N4 P5 113.31(5) . . . . ? N6 P4 N5 C35 140.93(15) . . . . ? N4 P4 N5 C35 -130.35(15) . . . . ? S4 P4 N5 C35 4.99(17) . . . . ? P5 P4 N5 C35 -174.92(13) . . . . ? O2 P5 N6 C39 89.83(14) . . . . ? N4 P5 N6 C39 -168.62(14) . . . . ? S5 P5 N6 C39 -44.54(15) . . . . ? P4 P5 N6 C39 -162.56(17) . . . . ? O2 P5 N6 P4 -107.61(6) . . . . ? N4 P5 N6 P4 -6.05(6) . . . . ? S5 P5 N6 P4 118.03(5) . . . . ? N5 P4 N6 C39 -83.00(15) . . . . ? N4 P4 N6 C39 168.08(15) . . . . ? S4 P4 N6 C39 50.50(15) . . . . ? P5 P4 N6 C39 162.18(17) . . . . ? N5 P4 N6 P5 114.82(7) . . . . ? N4 P4 N6 P5 5.91(6) . . . . ? S4 P4 N6 P5 -111.68(5) . . . . ? P5 N4 C31 C34 164.06(12) . . . . ? P4 N4 C31 C34 -42.0(2) . . . . ? P5 N4 C31 C32 45.25(19) . . . . ? P4 N4 C31 C32 -160.82(12) . . . . ? P5 N4 C31 C33 -75.37(18) . . . . ? P4 N4 C31 C33 78.56(17) . . . . ? P4 N5 C35 C38 56.2(2) . . . . ? P4 N5 C35 C37 -66.5(2) . . . . ? P4 N5 C35 C36 175.01(14) . . . . ? P5 N6 C39 C41 -158.02(12) . . . . ? P4 N6 C39 C41 45.46(19) . . . . ? P5 N6 C39 C42 -40.13(19) . . . . ? P4 N6 C39 C42 163.36(12) . . . . ? P5 N6 C39 C40 80.26(17) . . . . ? P4 N6 C39 C40 -76.26(18) . . . . ? P5 O2 C43 C44 -38.9(2) . . . . ? P5 O2 C43 C48 143.88(12) . . . . ? O2 C43 C44 C45 -179.56(15) . . . . ? C48 C43 C44 C45 -2.5(2) . . . . ? C43 C44 C45 C46 0.8(3) . . . . ? C44 C45 C46 C47 0.5(3) . . . . ? C45 C46 C47 C48 -0.2(3) . . . . ? C44 C43 C48 C47 2.8(2) . . . . ? O2 C43 C48 C47 -179.90(14) . . . . ? C44 C43 C48 P6 -176.88(13) . . . . ? O2 C43 C48 P6 0.37(19) . . . . ? C46 C47 C48 C43 -1.5(2) . . . . ? C46 C47 C48 P6 178.24(13) . . . . ? C49 P6 C48 C43 58.18(14) . . . . ? C55 P6 C48 C43 168.84(13) . . . . ? S6 P6 C48 C43 -68.26(14) . . . . ? C49 P6 C48 C47 -121.54(14) . . . . ? C55 P6 C48 C47 -10.88(15) . . . . ? S6 P6 C48 C47 112.02(13) . . . . ? C48 P6 C49 C54 -145.09(13) . . . . ? C55 P6 C49 C54 103.82(14) . . . . ? S6 P6 C49 C54 -18.13(15) . . . . ? C48 P6 C49 C50 38.01(16) . . . . ? C55 P6 C49 C50 -73.08(16) . . . . ? S6 P6 C49 C50 164.97(13) . . . . ? C54 C49 C50 C51 -2.2(3) . . . . ? P6 C49 C50 C51 174.74(16) . . . . ? C49 C50 C51 C52 1.7(3) . . . . ? C50 C51 C52 C53 0.3(3) . . . . ? C51 C52 C53 C54 -1.9(3) . . . . ? C50 C49 C54 C53 0.6(2) . . . . ? P6 C49 C54 C53 -176.36(12) . . . . ? C52 C53 C54 C49 1.5(3) . . . . ? C49 P6 C55 C56 -131.99(14) . . . . ? C48 P6 C55 C56 117.60(14) . . . . ? S6 P6 C55 C56 -7.90(15) . . . . ? C49 P6 C55 C60 45.18(16) . . . . ? C48 P6 C55 C60 -65.23(15) . . . . ? S6 P6 C55 C60 169.26(12) . . . . ? C60 C55 C56 C57 -0.7(3) . . . . ? P6 C55 C56 C57 176.59(15) . . . . ? C55 C56 C57 C58 0.9(3) . . . . ? C56 C57 C58 C59 -0.7(3) . . . . ? C57 C58 C59 C60 0.2(3) . . . . ? C58 C59 C60 C55 0.0(3) . . . . ? C56 C55 C60 C59 0.2(3) . . . . ? P6 C55 C60 C59 -176.91(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N S3 0.85 2.64 3.4617(14) 164 . N5 H5N S6 0.83 2.54 3.3554(14) 166 . _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.511 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.062 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 779801' #TrackingRef '- MSB-94.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tert-Butyl-[1,3-di-tert-butyl-4-(2-diphenyselenophosphorylphenoxy)- 2,4-diseleno-[1,3,2,4]diazadiphosphetidin-2-yl)amine ; _chemical_name_common ; tert-Butyl-(1,3-di-tert-butyl-4-(2- diphenyselenophosphorylphenoxy)-2,4-diseleno- (1,3,2,4)diazadiphosphetidin-2-yl)amine ; _chemical_melting_point ? _chemical_formula_moiety 'C30 H42 N3 O P3 Se3' _chemical_formula_sum 'C30 H42 N3 O P3 Se3' _chemical_formula_weight 790.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.091(1) _cell_length_b 15.017(1) _cell_length_c 16.446(1) _cell_angle_alpha 88.670(1) _cell_angle_beta 81.503(1) _cell_angle_gamma 89.306(1) _cell_volume 3440.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9774 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.28 _exptl_crystal_description Column _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 3.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4642 _exptl_absorpt_correction_T_max 0.5913 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60784 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.36 _reflns_number_total 16908 _reflns_number_gt 12284 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SMART (Bruker-AXS, 2000)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. ; _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _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^)+(0.0464P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16908 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 Se1 Se 0.86528(3) 0.37345(2) 1.13842(2) 0.02447(9) Uani 1 1 d . . . Se2 Se 0.72526(3) 0.49020(2) 0.89370(2) 0.02458(9) Uani 1 1 d . . . Se3 Se 0.78349(2) 0.07518(2) 0.88847(2) 0.02147(8) Uani 1 1 d . . . P1 P 0.80012(6) 0.30218(5) 1.05527(5) 0.01615(17) Uani 1 1 d . . . P2 P 0.73100(6) 0.35718(5) 0.93157(5) 0.01683(17) Uani 1 1 d . . . P3 P 0.75312(6) 0.01974(5) 1.00831(5) 0.01727(17) Uani 1 1 d . . . O1 O 0.78651(15) 0.19695(13) 1.07644(13) 0.0173(5) Uani 1 1 d . . . N1 N 0.69305(18) 0.33279(16) 1.03291(15) 0.0154(5) Uani 1 1 d . . . N2 N 0.83665(17) 0.31437(16) 0.95460(15) 0.0153(5) Uani 1 1 d . . . N3 N 0.68688(19) 0.28714(17) 0.87391(16) 0.0193(6) Uani 1 1 d . . . H3N H 0.6951 0.2266 0.8839 0.023 Uiso 1 1 d R . . C1 C 0.6041(2) 0.3583(2) 1.0889(2) 0.0209(7) Uani 1 1 d . . . C2 C 0.5193(2) 0.3533(2) 1.0415(2) 0.0256(8) Uani 1 1 d . . . H2A H 0.5275 0.3970 0.9958 0.038 Uiso 1 1 calc R . . H2B H 0.4598 0.3665 1.0783 0.038 Uiso 1 1 calc R . . H2C H 0.5161 0.2934 1.0199 0.038 Uiso 1 1 calc R . . C3 C 0.5918(3) 0.2908(2) 1.1614(2) 0.0281(8) Uani 1 1 d . . . H3A H 0.5910 0.2303 1.1405 0.042 Uiso 1 1 calc R . . H3B H 0.5313 0.3029 1.1973 0.042 Uiso 1 1 calc R . . H3C H 0.6453 0.2963 1.1928 0.042 Uiso 1 1 calc R . . C4 C 0.6114(3) 0.4522(2) 1.1204(2) 0.0307(8) Uani 1 1 d . . . H4A H 0.6699 0.4569 1.1457 0.046 Uiso 1 1 calc R . . H4B H 0.5553 0.4649 1.1614 0.046 Uiso 1 1 calc R . . H4C H 0.6138 0.4953 1.0745 0.046 Uiso 1 1 calc R . . C5 C 0.9363(2) 0.3155(2) 0.9079(2) 0.0208(7) Uani 1 1 d . . . C6 C 0.9941(2) 0.2428(2) 0.9462(2) 0.0236(7) Uani 1 1 d . . . H6A H 0.9964 0.2563 1.0039 0.035 Uiso 1 1 calc R . . H6B H 1.0595 0.2407 0.9161 0.035 Uiso 1 1 calc R . . H6C H 0.9634 0.1850 0.9430 0.035 Uiso 1 1 calc R . . C7 C 0.9822(2) 0.4069(2) 0.9128(2) 0.0280(8) Uani 1 1 d . . . H7A H 0.9420 0.4530 0.8915 0.042 Uiso 1 1 calc R . . H7B H 1.0461 0.4071 0.8799 0.042 Uiso 1 1 calc R . . H7C H 0.9879 0.4190 0.9702 0.042 Uiso 1 1 calc R . . C8 C 0.9309(2) 0.2930(2) 0.8188(2) 0.0236(7) Uani 1 1 d . . . H8A H 0.9027 0.2339 0.8168 0.035 Uiso 1 1 calc R . . H8B H 0.9956 0.2931 0.7873 0.035 Uiso 1 1 calc R . . H8C H 0.8909 0.3375 0.7951 0.035 Uiso 1 1 calc R . . C9 C 0.6345(2) 0.2964(2) 0.8002(2) 0.0231(7) Uani 1 1 d . . . C10 C 0.6014(3) 0.2030(2) 0.7841(2) 0.0408(10) Uani 1 1 d . . . H10A H 0.5674 0.2048 0.7363 0.061 Uiso 1 1 calc R . . H10B H 0.5583 0.1808 0.8324 0.061 Uiso 1 1 calc R . . H10C H 0.6574 0.1632 0.7734 0.061 Uiso 1 1 calc R . . C11 C 0.5472(3) 0.3571(3) 0.8182(2) 0.0347(9) Uani 1 1 d . . . H11A H 0.5148 0.3621 0.7695 0.052 Uiso 1 1 calc R . . H11B H 0.5675 0.4162 0.8323 0.052 Uiso 1 1 calc R . . H11C H 0.5029 0.3320 0.8644 0.052 Uiso 1 1 calc R . . C12 C 0.7016(3) 0.3297(3) 0.7258(2) 0.0344(9) Uani 1 1 d . . . H12A H 0.7584 0.2910 0.7168 0.052 Uiso 1 1 calc R . . H12B H 0.7211 0.3907 0.7349 0.052 Uiso 1 1 calc R . . H12C H 0.6687 0.3292 0.6773 0.052 Uiso 1 1 calc R . . C13 C 0.8468(2) 0.1325(2) 1.10474(19) 0.0168(6) Uani 1 1 d . . . C14 C 0.9083(2) 0.1501(2) 1.1605(2) 0.0254(8) Uani 1 1 d . . . H14 H 0.9117 0.2084 1.1809 0.030 Uiso 1 1 calc R . . C15 C 0.9651(2) 0.0815(2) 1.1866(2) 0.0262(8) Uani 1 1 d . . . H15 H 1.0081 0.0936 1.2243 0.031 Uiso 1 1 calc R . . C16 C 0.9594(2) -0.0036(2) 1.1581(2) 0.0269(8) Uani 1 1 d . . . H16 H 0.9984 -0.0501 1.1759 0.032 Uiso 1 1 calc R . . C17 C 0.8969(2) -0.0204(2) 1.1039(2) 0.0242(8) Uani 1 1 d . . . H17 H 0.8936 -0.0791 1.0842 0.029 Uiso 1 1 calc R . . C18 C 0.8380(2) 0.0461(2) 1.07663(19) 0.0179(7) Uani 1 1 d . . . C19 C 0.7528(2) -0.1022(2) 1.0054(2) 0.0226(7) Uani 1 1 d . . . C20 C 0.7125(3) -0.1540(2) 1.0725(2) 0.0294(8) Uani 1 1 d . . . H20 H 0.6857 -0.1261 1.1220 0.035 Uiso 1 1 calc R . . C21 C 0.7112(3) -0.2461(2) 1.0679(3) 0.0351(9) Uani 1 1 d . . . H21 H 0.6837 -0.2810 1.1141 0.042 Uiso 1 1 calc R . . C22 C 0.7496(3) -0.2866(3) 0.9965(3) 0.0458(11) Uani 1 1 d . . . H22 H 0.7481 -0.3496 0.9931 0.055 Uiso 1 1 calc R . . C23 C 0.7901(3) -0.2364(3) 0.9299(3) 0.0532(13) Uani 1 1 d . . . H23 H 0.8174 -0.2647 0.8807 0.064 Uiso 1 1 calc R . . C24 C 0.7912(3) -0.1440(2) 0.9345(3) 0.0367(9) Uani 1 1 d . . . H24 H 0.8187 -0.1094 0.8881 0.044 Uiso 1 1 calc R . . C25 C 0.6370(2) 0.0509(2) 1.0629(2) 0.0187(7) Uani 1 1 d . . . C26 C 0.5672(2) 0.0879(2) 1.0211(2) 0.0204(7) Uani 1 1 d . . . H26 H 0.5818 0.1007 0.9638 0.024 Uiso 1 1 calc R . . C27 C 0.4757(2) 0.1063(2) 1.0625(2) 0.0247(8) Uani 1 1 d . . . H27 H 0.4286 0.1330 1.0338 0.030 Uiso 1 1 calc R . . C28 C 0.4538(3) 0.0858(2) 1.1449(2) 0.0311(9) Uani 1 1 d . . . H28 H 0.3908 0.0966 1.1727 0.037 Uiso 1 1 calc R . . C29 C 0.5229(3) 0.0493(3) 1.1877(2) 0.0345(9) Uani 1 1 d . . . H29 H 0.5073 0.0348 1.2446 0.041 Uiso 1 1 calc R . . C30 C 0.6150(2) 0.0338(2) 1.1474(2) 0.0280(8) Uani 1 1 d . . . H30 H 0.6633 0.0116 1.1774 0.034 Uiso 1 1 calc R . . Se4 Se 0.58160(3) 0.89022(3) 0.60684(2) 0.03321(10) Uani 1 1 d . . . Se5 Se 0.53525(2) 0.67858(2) 0.39249(2) 0.02327(8) Uani 1 1 d . . . Se6 Se 0.97863(2) 0.74561(2) 0.404977(19) 0.01831(8) Uani 1 1 d . . . P4 P 0.68383(6) 0.80434(5) 0.54710(5) 0.01795(17) Uani 1 1 d . . . P5 P 0.66407(6) 0.69788(5) 0.43678(5) 0.01592(17) Uani 1 1 d . . . P6 P 0.99801(6) 0.76263(5) 0.52865(5) 0.01523(17) Uani 1 1 d . . . O2 O 0.78703(15) 0.80274(14) 0.57929(13) 0.0183(5) Uani 1 1 d . . . N4 N 0.66123(18) 0.69694(17) 0.54070(15) 0.0167(5) Uani 1 1 d . . . N5 N 0.70105(18) 0.80470(16) 0.44510(15) 0.0167(5) Uani 1 1 d . . . N6 N 0.75462(18) 0.63842(16) 0.39548(15) 0.0174(6) Uani 1 1 d . . . H6N H 0.8088 0.6588 0.4058 0.021 Uiso 1 1 d R . . C31 C 0.6179(2) 0.6317(2) 0.6064(2) 0.0235(7) Uani 1 1 d . . . C32 C 0.6413(3) 0.5386(2) 0.5753(2) 0.0301(8) Uani 1 1 d . . . H32A H 0.6119 0.5296 0.5258 0.045 Uiso 1 1 calc R . . H32B H 0.6161 0.4948 0.6179 0.045 Uiso 1 1 calc R . . H32C H 0.7111 0.5313 0.5622 0.045 Uiso 1 1 calc R . . C33 C 0.6639(2) 0.6480(2) 0.6833(2) 0.0271(8) Uani 1 1 d . . . H33A H 0.7337 0.6415 0.6700 0.041 Uiso 1 1 calc R . . H33B H 0.6396 0.6045 0.7265 0.041 Uiso 1 1 calc R . . H33C H 0.6479 0.7083 0.7026 0.041 Uiso 1 1 calc R . . C34 C 0.5095(2) 0.6454(3) 0.6245(2) 0.0313(9) Uani 1 1 d . . . H34A H 0.4953 0.7065 0.6427 0.047 Uiso 1 1 calc R . . H34B H 0.4824 0.6033 0.6679 0.047 Uiso 1 1 calc R . . H34C H 0.4812 0.6354 0.5746 0.047 Uiso 1 1 calc R . . C35 C 0.7104(2) 0.8813(2) 0.3844(2) 0.0216(7) Uani 1 1 d . . . C36 C 0.7576(2) 0.8470(2) 0.30152(19) 0.0247(8) Uani 1 1 d . . . H36A H 0.8192 0.8186 0.3077 0.037 Uiso 1 1 calc R . . H36B H 0.7683 0.8969 0.2619 0.037 Uiso 1 1 calc R . . H36C H 0.7156 0.8034 0.2817 0.037 Uiso 1 1 calc R . . C37 C 0.6124(3) 0.9231(2) 0.3769(2) 0.0320(9) Uani 1 1 d . . . H37A H 0.5714 0.8787 0.3571 0.048 Uiso 1 1 calc R . . H37B H 0.6207 0.9738 0.3380 0.048 Uiso 1 1 calc R . . H37C H 0.5823 0.9437 0.4308 0.048 Uiso 1 1 calc R . . C38 C 0.7746(3) 0.9497(2) 0.4157(2) 0.0295(8) Uani 1 1 d . . . H38A H 0.7434 0.9718 0.4688 0.044 Uiso 1 1 calc R . . H38B H 0.7855 0.9996 0.3760 0.044 Uiso 1 1 calc R . . H38C H 0.8362 0.9218 0.4226 0.044 Uiso 1 1 calc R . . C39 C 0.7679(2) 0.5690(2) 0.3297(2) 0.0200(7) Uani 1 1 d . . . C40 C 0.7560(3) 0.6105(2) 0.2468(2) 0.0261(8) Uani 1 1 d . . . H40A H 0.6906 0.6342 0.2489 0.039 Uiso 1 1 calc R . . H40B H 0.7677 0.5651 0.2045 0.039 Uiso 1 1 calc R . . H40C H 0.8021 0.6589 0.2335 0.039 Uiso 1 1 calc R . . C41 C 0.6987(3) 0.4919(2) 0.3517(2) 0.0291(8) Uani 1 1 d . . . H41A H 0.6325 0.5140 0.3551 0.044 Uiso 1 1 calc R . . H41B H 0.7086 0.4654 0.4048 0.044 Uiso 1 1 calc R . . H41C H 0.7105 0.4468 0.3092 0.044 Uiso 1 1 calc R . . C42 C 0.8700(2) 0.5342(2) 0.3283(2) 0.0274(8) Uani 1 1 d . . . H42A H 0.8840 0.4896 0.2855 0.041 Uiso 1 1 calc R . . H42B H 0.8766 0.5070 0.3819 0.041 Uiso 1 1 calc R . . H42C H 0.9150 0.5837 0.3165 0.041 Uiso 1 1 calc R . . C43 C 0.8439(2) 0.8721(2) 0.59985(19) 0.0176(7) Uani 1 1 d . . . C44 C 0.8055(2) 0.9441(2) 0.6444(2) 0.0215(7) Uani 1 1 d . . . H44 H 0.7385 0.9475 0.6631 0.026 Uiso 1 1 calc R . . C45 C 0.8656(3) 1.0115(2) 0.6615(2) 0.0235(7) Uani 1 1 d . . . H45 H 0.8396 1.0611 0.6924 0.028 Uiso 1 1 calc R . . C46 C 0.9629(2) 1.0072(2) 0.63388(19) 0.0207(7) Uani 1 1 d . . . H46 H 1.0033 1.0551 0.6426 0.025 Uiso 1 1 calc R . . C47 C 1.0011(2) 0.9321(2) 0.59327(19) 0.0205(7) Uani 1 1 d . . . H47 H 1.0684 0.9281 0.5764 0.025 Uiso 1 1 calc R . . C48 C 0.9431(2) 0.86247(19) 0.57665(19) 0.0161(6) Uani 1 1 d . . . C49 C 0.9525(2) 0.6715(2) 0.59724(19) 0.0173(7) Uani 1 1 d . . . C50 C 0.9388(2) 0.6813(2) 0.6825(2) 0.0218(7) Uani 1 1 d . . . H50 H 0.9490 0.7373 0.7053 0.026 Uiso 1 1 calc R . . C51 C 0.9103(2) 0.6084(2) 0.7338(2) 0.0264(8) Uani 1 1 d . . . H51 H 0.9016 0.6145 0.7918 0.032 Uiso 1 1 calc R . . C52 C 0.8945(2) 0.5274(2) 0.7003(2) 0.0268(8) Uani 1 1 d . . . H52 H 0.8752 0.4778 0.7357 0.032 Uiso 1 1 calc R . . C53 C 0.9064(2) 0.5174(2) 0.6163(2) 0.0261(8) Uani 1 1 d . . . H53 H 0.8947 0.4615 0.5939 0.031 Uiso 1 1 calc R . . C54 C 0.9353(2) 0.5894(2) 0.5645(2) 0.0201(7) Uani 1 1 d . . . H54 H 0.9436 0.5827 0.5066 0.024 Uiso 1 1 calc R . . C55 C 1.1247(2) 0.7716(2) 0.5378(2) 0.0192(7) Uani 1 1 d . . . C56 C 1.1594(3) 0.7524(2) 0.6117(2) 0.0284(8) Uani 1 1 d . . . H56 H 1.1170 0.7311 0.6581 0.034 Uiso 1 1 calc R . . C57 C 1.2556(3) 0.7646(3) 0.6175(2) 0.0343(9) Uani 1 1 d . . . H57 H 1.2787 0.7513 0.6678 0.041 Uiso 1 1 calc R . . C58 C 1.3181(3) 0.7959(2) 0.5502(2) 0.0310(9) Uani 1 1 d . . . H58 H 1.3839 0.8047 0.5543 0.037 Uiso 1 1 calc R . . C59 C 1.2843(3) 0.8141(3) 0.4775(2) 0.0337(9) Uani 1 1 d . . . H59 H 1.3269 0.8352 0.4311 0.040 Uiso 1 1 calc R . . C60 C 1.1887(2) 0.8018(2) 0.4712(2) 0.0273(8) Uani 1 1 d . . . H60 H 1.1664 0.8144 0.4204 0.033 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 Se1 0.03052(19) 0.01814(17) 0.02777(19) -0.00691(14) -0.01351(16) 0.00192(14) Se2 0.0335(2) 0.01241(16) 0.02819(19) 0.00372(13) -0.00659(16) 0.00381(14) Se3 0.02620(18) 0.01897(17) 0.01853(17) 0.00102(13) -0.00140(14) 0.00224(13) P1 0.0203(4) 0.0117(4) 0.0174(4) -0.0017(3) -0.0059(3) 0.0022(3) P2 0.0208(4) 0.0121(4) 0.0184(4) 0.0009(3) -0.0056(3) 0.0025(3) P3 0.0185(4) 0.0132(4) 0.0203(4) 0.0002(3) -0.0037(3) 0.0023(3) O1 0.0215(12) 0.0112(11) 0.0207(12) 0.0003(9) -0.0083(10) 0.0028(9) N1 0.0177(13) 0.0138(13) 0.0153(13) -0.0005(10) -0.0042(11) 0.0032(10) N2 0.0162(13) 0.0120(13) 0.0180(14) 0.0004(10) -0.0039(11) 0.0046(10) N3 0.0274(15) 0.0114(13) 0.0207(14) 0.0015(11) -0.0093(12) 0.0024(11) C1 0.0245(17) 0.0187(17) 0.0187(17) -0.0061(13) -0.0005(14) 0.0067(13) C2 0.0207(17) 0.032(2) 0.0244(19) -0.0013(15) -0.0048(15) 0.0051(14) C3 0.030(2) 0.033(2) 0.0214(18) -0.0022(15) -0.0031(16) 0.0042(16) C4 0.031(2) 0.027(2) 0.035(2) -0.0122(16) -0.0073(17) 0.0107(16) C5 0.0205(17) 0.0149(16) 0.0265(18) 0.0014(13) -0.0022(14) -0.0002(13) C6 0.0194(17) 0.0220(18) 0.0279(19) 0.0014(14) 0.0006(15) 0.0041(13) C7 0.0273(19) 0.0204(18) 0.036(2) -0.0021(15) -0.0017(16) -0.0031(14) C8 0.0225(18) 0.0204(18) 0.0261(19) 0.0018(14) 0.0017(15) 0.0011(14) C9 0.0284(19) 0.0222(18) 0.0213(17) -0.0008(14) -0.0126(15) 0.0041(14) C10 0.059(3) 0.030(2) 0.042(2) 0.0066(18) -0.037(2) -0.0068(19) C11 0.032(2) 0.048(2) 0.027(2) -0.0090(17) -0.0153(17) 0.0129(18) C12 0.038(2) 0.045(2) 0.0220(19) 0.0003(17) -0.0112(17) 0.0028(18) C13 0.0164(15) 0.0173(16) 0.0157(16) 0.0009(12) 0.0006(13) 0.0040(12) C14 0.032(2) 0.0221(18) 0.0238(18) 0.0009(14) -0.0114(16) 0.0049(15) C15 0.031(2) 0.0249(19) 0.0253(19) 0.0045(15) -0.0132(16) 0.0025(15) C16 0.0221(18) 0.0210(18) 0.039(2) 0.0084(15) -0.0110(16) 0.0018(14) C17 0.0219(17) 0.0168(17) 0.034(2) 0.0005(14) -0.0057(15) 0.0048(13) C18 0.0133(15) 0.0182(16) 0.0222(17) 0.0030(13) -0.0029(13) 0.0005(12) C19 0.0216(17) 0.0154(16) 0.032(2) -0.0017(14) -0.0095(15) 0.0027(13) C20 0.037(2) 0.0187(18) 0.035(2) 0.0053(15) -0.0160(17) -0.0015(15) C21 0.042(2) 0.0186(19) 0.049(3) 0.0087(17) -0.023(2) -0.0074(16) C22 0.057(3) 0.0150(19) 0.072(3) -0.003(2) -0.028(3) -0.0028(18) C23 0.072(3) 0.025(2) 0.059(3) -0.015(2) 0.005(3) 0.005(2) C24 0.039(2) 0.0212(19) 0.046(2) -0.0074(17) 0.006(2) -0.0011(16) C25 0.0165(16) 0.0157(16) 0.0227(17) -0.0005(13) 0.0008(14) 0.0016(12) C26 0.0246(17) 0.0144(16) 0.0231(18) -0.0032(13) -0.0067(14) 0.0010(13) C27 0.0210(18) 0.0207(18) 0.034(2) -0.0054(15) -0.0076(16) 0.0024(14) C28 0.0207(18) 0.034(2) 0.036(2) -0.0033(17) 0.0039(16) 0.0040(15) C29 0.030(2) 0.043(2) 0.027(2) 0.0053(17) 0.0062(17) 0.0058(17) C30 0.0248(19) 0.033(2) 0.0260(19) 0.0033(15) -0.0046(15) 0.0070(15) Se4 0.02250(19) 0.0406(2) 0.0378(2) -0.01991(18) -0.00679(17) 0.01196(16) Se5 0.01810(17) 0.02833(19) 0.02519(19) -0.00163(14) -0.00891(14) -0.00142(14) Se6 0.02192(17) 0.01595(16) 0.01795(16) -0.00032(12) -0.00586(13) -0.00123(12) P4 0.0161(4) 0.0187(4) 0.0196(4) -0.0038(3) -0.0040(3) 0.0020(3) P5 0.0163(4) 0.0153(4) 0.0166(4) 0.0000(3) -0.0039(3) -0.0007(3) P6 0.0176(4) 0.0121(4) 0.0165(4) 0.0009(3) -0.0044(3) -0.0004(3) O2 0.0175(11) 0.0164(11) 0.0219(12) -0.0034(9) -0.0054(10) -0.0016(9) N4 0.0176(13) 0.0184(14) 0.0145(13) 0.0008(11) -0.0034(11) -0.0040(11) N5 0.0197(14) 0.0132(13) 0.0179(14) -0.0002(10) -0.0050(11) -0.0011(10) N6 0.0157(13) 0.0172(14) 0.0205(14) -0.0044(11) -0.0055(11) -0.0001(10) C31 0.0219(18) 0.0292(19) 0.0190(17) 0.0045(14) -0.0026(14) -0.0064(14) C32 0.036(2) 0.0258(19) 0.028(2) 0.0091(15) -0.0041(17) -0.0104(16) C33 0.0249(18) 0.036(2) 0.0210(18) 0.0061(15) -0.0058(15) -0.0067(15) C34 0.0205(18) 0.047(2) 0.026(2) 0.0051(17) -0.0019(16) -0.0086(16) C35 0.0250(18) 0.0159(16) 0.0248(18) 0.0062(13) -0.0075(15) 0.0000(13) C36 0.033(2) 0.0206(18) 0.0207(17) 0.0063(14) -0.0063(15) -0.0018(15) C37 0.033(2) 0.0255(19) 0.040(2) 0.0056(16) -0.0147(18) 0.0059(16) C38 0.036(2) 0.0194(18) 0.035(2) 0.0042(15) -0.0120(17) -0.0013(15) C39 0.0227(17) 0.0140(16) 0.0247(18) -0.0034(13) -0.0075(14) -0.0012(13) C40 0.033(2) 0.0260(19) 0.0200(18) -0.0054(14) -0.0041(16) 0.0017(15) C41 0.033(2) 0.0181(18) 0.036(2) -0.0035(15) -0.0050(17) -0.0063(15) C42 0.0270(19) 0.0245(19) 0.032(2) -0.0119(15) -0.0061(16) 0.0050(15) C43 0.0259(17) 0.0118(15) 0.0160(16) -0.0006(12) -0.0063(14) -0.0010(13) C44 0.0242(18) 0.0213(17) 0.0195(17) -0.0044(13) -0.0040(14) 0.0031(14) C45 0.037(2) 0.0145(16) 0.0189(17) -0.0031(13) -0.0051(16) 0.0043(14) C46 0.0308(19) 0.0099(15) 0.0228(17) 0.0005(13) -0.0084(15) -0.0064(13) C47 0.0235(17) 0.0184(17) 0.0197(17) 0.0033(13) -0.0040(14) -0.0017(13) C48 0.0222(16) 0.0104(15) 0.0173(16) 0.0025(12) -0.0079(13) -0.0021(12) C49 0.0146(15) 0.0167(16) 0.0205(17) 0.0025(13) -0.0027(13) 0.0000(12) C50 0.0221(17) 0.0192(17) 0.0244(18) 0.0015(14) -0.0044(15) 0.0008(13) C51 0.0216(18) 0.031(2) 0.0253(19) 0.0085(15) 0.0000(15) 0.0036(15) C52 0.0249(18) 0.0202(18) 0.034(2) 0.0146(15) -0.0014(16) 0.0013(14) C53 0.0230(18) 0.0162(17) 0.039(2) 0.0057(15) -0.0042(16) 0.0015(13) C54 0.0189(16) 0.0144(16) 0.0266(18) 0.0009(13) -0.0021(14) 0.0000(12) C55 0.0180(16) 0.0149(16) 0.0254(18) 0.0000(13) -0.0059(14) -0.0017(12) C56 0.0280(19) 0.033(2) 0.0249(19) 0.0051(15) -0.0077(16) -0.0025(16) C57 0.029(2) 0.042(2) 0.035(2) 0.0077(18) -0.0174(18) -0.0024(17) C58 0.0199(18) 0.032(2) 0.044(2) -0.0026(17) -0.0144(17) -0.0009(15) C59 0.0227(19) 0.042(2) 0.036(2) 0.0018(18) -0.0008(17) -0.0060(16) C60 0.0220(18) 0.035(2) 0.0251(19) 0.0030(15) -0.0046(15) -0.0046(15) _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 Se1 P1 2.0789(9) . ? Se2 P2 2.0828(8) . ? Se3 P3 2.1081(9) . ? P1 O1 1.618(2) . ? P1 N1 1.662(3) . ? P1 N2 1.666(3) . ? P2 N3 1.621(3) . ? P2 N2 1.704(2) . ? P2 N1 1.706(3) . ? P3 C25 1.808(3) . ? P3 C18 1.811(3) . ? P3 C19 1.833(3) . ? O1 C13 1.398(3) . ? N1 C1 1.493(4) . ? N2 C5 1.498(4) . ? N3 C9 1.513(4) . ? N3 H3N 0.9294 . ? C1 C2 1.522(4) . ? C1 C4 1.524(4) . ? C1 C3 1.540(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.525(4) . ? C5 C6 1.532(4) . ? C5 C7 1.533(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C12 1.511(5) . ? C9 C11 1.520(5) . ? C9 C10 1.524(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.383(4) . ? C13 C18 1.400(4) . ? C14 C15 1.395(4) . ? C14 H14 0.9500 . ? C15 C16 1.379(5) . ? C15 H15 0.9500 . ? C16 C17 1.372(5) . ? C16 H16 0.9500 . ? C17 C18 1.400(4) . ? C17 H17 0.9500 . ? C19 C24 1.373(5) . ? C19 C20 1.390(5) . ? C20 C21 1.387(5) . ? C20 H20 0.9500 . ? C21 C22 1.371(6) . ? C21 H21 0.9500 . ? C22 C23 1.371(6) . ? C22 H22 0.9500 . ? C23 C24 1.392(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.385(4) . ? C25 C30 1.397(4) . ? C26 C27 1.394(4) . ? C26 H26 0.9500 . ? C27 C28 1.373(5) . ? C27 H27 0.9500 . ? C28 C29 1.385(5) . ? C28 H28 0.9500 . ? C29 C30 1.386(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? Se4 P4 2.0735(9) . ? Se5 P5 2.0790(9) . ? Se6 P6 2.1135(9) . ? P4 O2 1.619(2) . ? P4 N4 1.656(3) . ? P4 N5 1.659(3) . ? P5 N6 1.622(3) . ? P5 N4 1.703(3) . ? P5 N5 1.707(3) . ? P6 C49 1.815(3) . ? P6 C55 1.821(3) . ? P6 C48 1.821(3) . ? O2 C43 1.399(4) . ? N4 C31 1.507(4) . ? N5 C35 1.500(4) . ? N6 C39 1.509(4) . ? N6 H6N 0.8665 . ? C31 C32 1.516(5) . ? C31 C34 1.525(5) . ? C31 C33 1.529(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.524(5) . ? C35 C38 1.525(5) . ? C35 C37 1.531(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.516(4) . ? C39 C42 1.522(4) . ? C39 C41 1.525(4) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.380(4) . ? C43 C48 1.401(4) . ? C44 C45 1.388(4) . ? C44 H44 0.9500 . ? C45 C46 1.380(5) . ? C45 H45 0.9500 . ? C46 C47 1.386(4) . ? C46 H46 0.9500 . ? C47 C48 1.391(4) . ? C47 H47 0.9500 . ? C49 C54 1.394(4) . ? C49 C50 1.398(4) . ? C50 C51 1.393(4) . ? C50 H50 0.9500 . ? C51 C52 1.382(5) . ? C51 H51 0.9500 . ? C52 C53 1.379(5) . ? C52 H52 0.9500 . ? C53 C54 1.387(4) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.383(5) . ? C55 C56 1.398(4) . ? C56 C57 1.387(5) . ? C56 H56 0.9500 . ? C57 C58 1.386(5) . ? C57 H57 0.9500 . ? C58 C59 1.371(5) . ? C58 H58 0.9500 . ? C59 C60 1.381(5) . ? C59 H59 0.9500 . ? C60 H60 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 O1 P1 N1 102.62(12) . . ? O1 P1 N2 108.14(12) . . ? N1 P1 N2 85.07(12) . . ? O1 P1 Se1 115.43(8) . . ? N1 P1 Se1 120.63(10) . . ? N2 P1 Se1 120.21(10) . . ? N3 P2 N2 108.15(13) . . ? N3 P2 N1 110.39(13) . . ? N2 P2 N1 82.55(12) . . ? N3 P2 Se2 115.14(10) . . ? N2 P2 Se2 118.96(9) . . ? N1 P2 Se2 117.25(9) . . ? C25 P3 C18 105.15(15) . . ? C25 P3 C19 105.46(15) . . ? C18 P3 C19 105.16(14) . . ? C25 P3 Se3 114.27(11) . . ? C18 P3 Se3 115.31(11) . . ? C19 P3 Se3 110.61(12) . . ? C13 O1 P1 132.3(2) . . ? C1 N1 P1 129.7(2) . . ? C1 N1 P2 131.6(2) . . ? P1 N1 P2 95.92(13) . . ? C5 N2 P1 129.7(2) . . ? C5 N2 P2 131.8(2) . . ? P1 N2 P2 95.83(13) . . ? C9 N3 P2 134.3(2) . . ? C9 N3 H3N 107.2 . . ? P2 N3 H3N 118.5 . . ? N1 C1 C2 108.5(3) . . ? N1 C1 C4 111.1(3) . . ? C2 C1 C4 109.8(3) . . ? N1 C1 C3 107.3(2) . . ? C2 C1 C3 110.1(3) . . ? C4 C1 C3 109.9(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C8 108.3(3) . . ? N2 C5 C6 107.3(2) . . ? C8 C5 C6 109.2(3) . . ? N2 C5 C7 110.7(3) . . ? C8 C5 C7 110.6(3) . . ? C6 C5 C7 110.6(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C9 N3 110.4(3) . . ? C12 C9 C11 111.0(3) . . ? N3 C9 C11 111.1(3) . . ? C12 C9 C10 109.1(3) . . ? N3 C9 C10 105.9(3) . . ? C11 C9 C10 109.1(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 O1 123.1(3) . . ? C14 C13 C18 120.9(3) . . ? O1 C13 C18 115.8(3) . . ? C13 C14 C15 119.5(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 120.5(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 119.3(3) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 122.1(3) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C17 C18 C13 117.5(3) . . ? C17 C18 P3 120.5(3) . . ? C13 C18 P3 122.0(2) . . ? C24 C19 C20 118.7(3) . . ? C24 C19 P3 119.5(3) . . ? C20 C19 P3 121.8(3) . . ? C21 C20 C19 120.6(4) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 119.9(4) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 120.2(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 119.9(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C19 C24 C23 120.8(4) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C26 C25 C30 119.2(3) . . ? C26 C25 P3 120.5(2) . . ? C30 C25 P3 120.2(2) . . ? C25 C26 C27 120.3(3) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 120.0(3) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.3(3) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C30 120.0(3) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 120.1(3) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? O2 P4 N4 102.40(12) . . ? O2 P4 N5 109.03(12) . . ? N4 P4 N5 85.33(13) . . ? O2 P4 Se4 115.94(9) . . ? N4 P4 Se4 120.93(10) . . ? N5 P4 Se4 118.56(10) . . ? N6 P5 N4 109.18(13) . . ? N6 P5 N5 108.87(13) . . ? N4 P5 N5 82.41(12) . . ? N6 P5 Se5 116.09(10) . . ? N4 P5 Se5 117.46(9) . . ? N5 P5 Se5 118.04(9) . . ? C49 P6 C55 105.96(14) . . ? C49 P6 C48 104.97(14) . . ? C55 P6 C48 104.52(14) . . ? C49 P6 Se6 113.95(11) . . ? C55 P6 Se6 111.07(11) . . ? C48 P6 Se6 115.48(10) . . ? C43 O2 P4 130.97(19) . . ? C31 N4 P4 129.8(2) . . ? C31 N4 P5 131.1(2) . . ? P4 N4 P5 95.85(13) . . ? C35 N5 P4 130.1(2) . . ? C35 N5 P5 131.0(2) . . ? P4 N5 P5 95.60(13) . . ? C39 N6 P5 134.0(2) . . ? C39 N6 H6N 112.4 . . ? P5 N6 H6N 112.1 . . ? N4 C31 C32 107.8(3) . . ? N4 C31 C34 110.3(3) . . ? C32 C31 C34 110.2(3) . . ? N4 C31 C33 107.4(3) . . ? C32 C31 C33 110.6(3) . . ? C34 C31 C33 110.5(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N5 C35 C36 108.2(3) . . ? N5 C35 C38 106.9(3) . . ? C36 C35 C38 110.1(3) . . ? N5 C35 C37 111.2(3) . . ? C36 C35 C37 110.4(3) . . ? C38 C35 C37 109.9(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N6 C39 C40 110.6(2) . . ? N6 C39 C42 105.2(2) . . ? C40 C39 C42 110.1(3) . . ? N6 C39 C41 111.1(3) . . ? C40 C39 C41 110.9(3) . . ? C42 C39 C41 108.7(3) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 O2 122.2(3) . . ? C44 C43 C48 121.3(3) . . ? O2 C43 C48 116.4(3) . . ? C43 C44 C45 119.4(3) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C46 C45 C44 120.5(3) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 119.3(3) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 120.3 . . ? C46 C47 C48 121.6(3) . . ? C46 C47 H47 119.2 . . ? C48 C47 H47 119.2 . . ? C47 C48 C43 117.6(3) . . ? C47 C48 P6 119.6(2) . . ? C43 C48 P6 122.8(2) . . ? C54 C49 C50 119.7(3) . . ? C54 C49 P6 119.5(2) . . ? C50 C49 P6 120.8(2) . . ? C51 C50 C49 119.6(3) . . ? C51 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? C52 C51 C50 120.0(3) . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C53 C52 C51 120.8(3) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C52 C53 C54 119.7(3) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C53 C54 C49 120.2(3) . . ? C53 C54 H54 119.9 . . ? C49 C54 H54 119.9 . . ? C60 C55 C56 118.4(3) . . ? C60 C55 P6 119.6(2) . . ? C56 C55 P6 121.9(3) . . ? C57 C56 C55 120.2(3) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C58 C57 C56 120.4(3) . . ? C58 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C59 C58 C57 119.4(3) . . ? C59 C58 H58 120.3 . . ? C57 C58 H58 120.3 . . ? C58 C59 C60 120.5(4) . . ? C58 C59 H59 119.8 . . ? C60 C59 H59 119.8 . . ? C59 C60 C55 121.1(3) . . ? C59 C60 H60 119.4 . . ? C55 C60 H60 119.4 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.838 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.112 #===END data_11 _database_code_depnum_ccdc_archive 'CCDC 779802' #TrackingRef '- MSB-94.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H46 Cl2 N2 O4 P4 Rh2, C H2 Cl2' _chemical_formula_sum 'C47 H48 Cl4 N2 O4 P4 Rh2' _chemical_formula_weight 1176.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3543(8) _cell_length_b 28.627(2) _cell_length_c 17.0271(13) _cell_angle_alpha 90.00 _cell_angle_beta 100.523(1) _cell_angle_gamma 90.00 _cell_volume 4962.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3871 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.48 _exptl_crystal_description Column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 1.054 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8058 _exptl_absorpt_correction_T_max 0.9299 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 20 sec/frame. Inspection of 2199 reflections harvested from the full data set and having I/\s(I) > 15 with CELL_NOW (Sheldrick, 2008) indicated that the crystal was twinned by a rotation of the primitive monoclinc cell of 180 deg. about a. Integration of the 2-component raw data was accomplished with the multi-component version of SAINT under control of the 2-component orientation file generated by CELL_NOW. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 82526 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.61 _reflns_number_total 11473 _reflns_number_gt 9225 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS, 2008)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2008a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2008a)' _publ_section_references ; Bruker-AXS (2006). APEX2, Version 2.1-0, Madison, WI. Bruker-AXS (2008). SAINT, Version 7.53A, Madison, WI Bruker-AXS (2008a). SHELXTL, Version 2008/3, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008). CELL_NOW Version 2008/2. University of G\"ottingen, Germany. Sheldrick, G, M. (2008a). TWINABS, Version 2008/4. University of G\"ottingen, Germany. ; _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. Trial refinements of the model obtained using the single-component reflection data extracted from the full data set by TWINABS with that obtained using the full 2-component reflection file indicated the former to be superior. ; _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^)+(0.0164P)^2^+11.6664P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 11473 _refine_ls_number_parameters 574 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Rh1 Rh 0.41732(2) 0.097468(8) 0.740513(14) 0.01327(6) Uani 1 1 d . . . Rh2 Rh 0.12018(2) 0.277140(8) 0.659440(14) 0.01503(6) Uani 1 1 d . . . Cl1 Cl 0.62057(7) 0.06119(3) 0.72941(5) 0.01999(16) Uani 1 1 d . . . Cl2 Cl 0.13352(8) 0.35644(3) 0.62287(5) 0.02178(16) Uani 1 1 d . . . P1 P 0.33241(7) 0.02343(3) 0.75363(5) 0.01476(15) Uani 1 1 d . . . P2 P 0.22560(7) 0.12949(3) 0.73082(5) 0.01331(15) Uani 1 1 d . . . P3 P 0.10413(7) 0.20525(3) 0.69623(5) 0.01454(15) Uani 1 1 d . . . P4 P -0.10727(7) 0.28534(3) 0.63527(5) 0.01484(16) Uani 1 1 d . . . O1 O 0.10233(19) 0.09425(7) 0.73476(13) 0.0186(5) Uani 1 1 d . . . O2 O -0.0439(2) 0.19076(7) 0.71131(13) 0.0176(4) Uani 1 1 d . . . O3 O 0.5524(2) 0.19156(8) 0.74544(16) 0.0325(6) Uani 1 1 d . . . O4 O 0.4155(3) 0.27679(11) 0.6905(3) 0.0699(12) Uani 1 1 d . . . N1 N 0.1560(2) 0.15932(8) 0.64795(14) 0.0148(5) Uani 1 1 d . . . N2 N 0.1940(2) 0.17960(9) 0.77736(15) 0.0160(5) Uani 1 1 d . . . C1 C 0.4445(3) -0.01563(11) 0.81669(18) 0.0166(6) Uani 1 1 d . . . C2 C 0.4512(3) -0.06327(11) 0.8002(2) 0.0217(7) Uani 1 1 d . . . H2 H 0.3973 -0.0763 0.7543 0.026 Uiso 1 1 calc R . . C3 C 0.5377(3) -0.09159(12) 0.8517(2) 0.0285(8) Uani 1 1 d . . . H3 H 0.5432 -0.1240 0.8405 0.034 Uiso 1 1 calc R . . C4 C 0.6151(3) -0.07290(14) 0.9187(2) 0.0306(8) Uani 1 1 d . . . H4 H 0.6739 -0.0924 0.9534 0.037 Uiso 1 1 calc R . . C5 C 0.6075(3) -0.02575(13) 0.9356(2) 0.0282(8) Uani 1 1 d . . . H5 H 0.6605 -0.0131 0.9822 0.034 Uiso 1 1 calc R . . C6 C 0.5226(3) 0.00290(12) 0.88460(19) 0.0228(7) Uani 1 1 d . . . H6 H 0.5178 0.0353 0.8961 0.027 Uiso 1 1 calc R . . C7 C 0.2900(3) -0.00484(10) 0.65647(19) 0.0199(7) Uani 1 1 d . . . C8 C 0.1603(3) -0.01501(12) 0.6237(2) 0.0282(8) Uani 1 1 d . . . H8 H 0.0930 -0.0096 0.6537 0.034 Uiso 1 1 calc R . . C9 C 0.1292(4) -0.03316(13) 0.5468(2) 0.0386(10) Uani 1 1 d . . . H9 H 0.0404 -0.0403 0.5246 0.046 Uiso 1 1 calc R . . C10 C 0.2250(5) -0.04076(13) 0.5028(2) 0.0407(10) Uani 1 1 d . . . H10 H 0.2028 -0.0529 0.4502 0.049 Uiso 1 1 calc R . . C11 C 0.3541(5) -0.03072(14) 0.5350(2) 0.0411(10) Uani 1 1 d . . . H11 H 0.4207 -0.0363 0.5045 0.049 Uiso 1 1 calc R . . C12 C 0.3875(4) -0.01263(12) 0.6113(2) 0.0288(8) Uani 1 1 d . . . H12 H 0.4765 -0.0055 0.6328 0.035 Uiso 1 1 calc R . . C13 C 0.1849(3) 0.02069(11) 0.79671(19) 0.0183(6) Uani 1 1 d . . . C14 C 0.1589(3) -0.01761(12) 0.8435(2) 0.0255(7) Uani 1 1 d . . . H14 H 0.2207 -0.0424 0.8533 0.031 Uiso 1 1 calc R . . C15 C 0.0457(4) -0.01997(13) 0.8754(2) 0.0320(8) Uani 1 1 d . . . H15 H 0.0301 -0.0461 0.9068 0.038 Uiso 1 1 calc R . . C16 C -0.0447(3) 0.01596(13) 0.8614(2) 0.0310(8) Uani 1 1 d . . . H16 H -0.1229 0.0144 0.8831 0.037 Uiso 1 1 calc R . . C17 C -0.0223(3) 0.05417(12) 0.8160(2) 0.0249(7) Uani 1 1 d . . . H17 H -0.0847 0.0788 0.8066 0.030 Uiso 1 1 calc R . . C18 C 0.0924(3) 0.05636(11) 0.78416(19) 0.0184(6) Uani 1 1 d . . . C19 C 0.4991(3) 0.15711(11) 0.74082(19) 0.0196(7) Uani 1 1 d . . . C20 C 0.1643(3) 0.15217(11) 0.56247(18) 0.0169(6) Uani 1 1 d . . . C21 C 0.1789(4) 0.09999(12) 0.5491(2) 0.0349(9) Uani 1 1 d . . . H21A H 0.1058 0.0833 0.5657 0.052 Uiso 1 1 calc R . . H21B H 0.2621 0.0890 0.5806 0.052 Uiso 1 1 calc R . . H21C H 0.1782 0.0941 0.4923 0.052 Uiso 1 1 calc R . . C22 C 0.0382(3) 0.17012(13) 0.51097(19) 0.0257(7) Uani 1 1 d . . . H22A H 0.0443 0.1671 0.4544 0.039 Uiso 1 1 calc R . . H22B H 0.0256 0.2030 0.5235 0.039 Uiso 1 1 calc R . . H22C H -0.0365 0.1518 0.5218 0.039 Uiso 1 1 calc R . . C23 C 0.2826(3) 0.17808(14) 0.5425(2) 0.0312(8) Uani 1 1 d . . . H23A H 0.2896 0.1719 0.4869 0.047 Uiso 1 1 calc R . . H23B H 0.3625 0.1673 0.5779 0.047 Uiso 1 1 calc R . . H23C H 0.2718 0.2117 0.5501 0.047 Uiso 1 1 calc R . . C24 C 0.2142(3) 0.19154(12) 0.86421(19) 0.0235(7) Uani 1 1 d . . . C25 C 0.1755(4) 0.14938(13) 0.9095(2) 0.0386(10) Uani 1 1 d . . . H25A H 0.0844 0.1407 0.8878 0.058 Uiso 1 1 calc R . . H25B H 0.1836 0.1572 0.9662 0.058 Uiso 1 1 calc R . . H25C H 0.2336 0.1231 0.9036 0.058 Uiso 1 1 calc R . . C26 C 0.3567(4) 0.20460(19) 0.8938(3) 0.0532(13) Uani 1 1 d . . . H26A H 0.4130 0.1778 0.8876 0.080 Uiso 1 1 calc R . . H26B H 0.3690 0.2134 0.9503 0.080 Uiso 1 1 calc R . . H26C H 0.3802 0.2310 0.8625 0.080 Uiso 1 1 calc R . . C27 C 0.1249(4) 0.23242(13) 0.8752(2) 0.0304(8) Uani 1 1 d . . . H27A H 0.1497 0.2598 0.8466 0.046 Uiso 1 1 calc R . . H27B H 0.1342 0.2397 0.9322 0.046 Uiso 1 1 calc R . . H27C H 0.0335 0.2241 0.8538 0.046 Uiso 1 1 calc R . . C28 C -0.1547(3) 0.19081(11) 0.65115(18) 0.0173(6) Uani 1 1 d . . . C29 C -0.2212(3) 0.14896(11) 0.6352(2) 0.0217(7) Uani 1 1 d . . . H29 H -0.1894 0.1214 0.6634 0.026 Uiso 1 1 calc R . . C30 C -0.3348(3) 0.14764(12) 0.5777(2) 0.0241(7) Uani 1 1 d . . . H30 H -0.3818 0.1192 0.5667 0.029 Uiso 1 1 calc R . . C31 C -0.3799(3) 0.18791(12) 0.5360(2) 0.0243(7) Uani 1 1 d . . . H31 H -0.4571 0.1868 0.4961 0.029 Uiso 1 1 calc R . . C32 C -0.3129(3) 0.22943(11) 0.55259(19) 0.0203(7) Uani 1 1 d . . . H32 H -0.3442 0.2568 0.5236 0.024 Uiso 1 1 calc R . . C33 C -0.2000(3) 0.23187(10) 0.61126(18) 0.0162(6) Uani 1 1 d . . . C34 C -0.1761(3) 0.32396(11) 0.55375(19) 0.0178(6) Uani 1 1 d . . . C35 C -0.1446(3) 0.31600(12) 0.4791(2) 0.0255(7) Uani 1 1 d . . . H35 H -0.0866 0.2913 0.4721 0.031 Uiso 1 1 calc R . . C36 C -0.1972(3) 0.34390(13) 0.4146(2) 0.0295(8) Uani 1 1 d . . . H36 H -0.1762 0.3380 0.3634 0.035 Uiso 1 1 calc R . . C37 C -0.2802(4) 0.38025(13) 0.4248(2) 0.0304(8) Uani 1 1 d . . . H37 H -0.3153 0.3996 0.3808 0.036 Uiso 1 1 calc R . . C38 C -0.3122(4) 0.38849(13) 0.4985(2) 0.0307(8) Uani 1 1 d . . . H38 H -0.3694 0.4135 0.5053 0.037 Uiso 1 1 calc R . . C39 C -0.2608(3) 0.36023(12) 0.5631(2) 0.0245(7) Uani 1 1 d . . . H39 H -0.2837 0.3658 0.6139 0.029 Uiso 1 1 calc R . . C40 C -0.1622(3) 0.30858(11) 0.72277(18) 0.0166(6) Uani 1 1 d . . . C41 C -0.0977(3) 0.34752(12) 0.7607(2) 0.0244(7) Uani 1 1 d . . . H41 H -0.0246 0.3605 0.7418 0.029 Uiso 1 1 calc R . . C42 C -0.1400(4) 0.36727(12) 0.8255(2) 0.0279(8) Uani 1 1 d . . . H42 H -0.0962 0.3940 0.8506 0.033 Uiso 1 1 calc R . . C43 C -0.2447(4) 0.34871(14) 0.8541(2) 0.0306(8) Uani 1 1 d . . . H43 H -0.2730 0.3625 0.8988 0.037 Uiso 1 1 calc R . . C44 C -0.3080(4) 0.31021(16) 0.8179(2) 0.0414(10) Uani 1 1 d . . . H44 H -0.3800 0.2972 0.8378 0.050 Uiso 1 1 calc R . . C45 C -0.2675(3) 0.29004(14) 0.7519(2) 0.0317(8) Uani 1 1 d . . . H45 H -0.3123 0.2635 0.7269 0.038 Uiso 1 1 calc R . . C46 C 0.3057(4) 0.27512(12) 0.6797(3) 0.0341(9) Uani 1 1 d . . . C47 C 0.2692(4) 0.43109(14) 0.7864(2) 0.0333(8) Uani 1 1 d . . . H47A H 0.3276 0.4559 0.7725 0.040 Uiso 1 1 calc R . . H47B H 0.2216 0.4173 0.7360 0.040 Uiso 1 1 calc R . . Cl3 Cl 0.36470(13) 0.38755(5) 0.84311(8) 0.0640(4) Uani 1 1 d . . . Cl4 Cl 0.15701(14) 0.45532(5) 0.83877(8) 0.0698(4) Uani 1 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 Rh1 0.01185(11) 0.01099(11) 0.01706(11) 0.00027(9) 0.00285(8) 0.00066(9) Rh2 0.01258(11) 0.01103(11) 0.02142(12) 0.00097(9) 0.00297(9) 0.00002(9) Cl1 0.0145(3) 0.0167(4) 0.0297(4) 0.0008(3) 0.0064(3) 0.0020(3) Cl2 0.0226(4) 0.0133(4) 0.0298(4) 0.0028(3) 0.0056(3) -0.0023(3) P1 0.0127(3) 0.0120(4) 0.0195(4) 0.0009(3) 0.0027(3) 0.0011(3) P2 0.0135(3) 0.0104(4) 0.0160(4) 0.0007(3) 0.0029(3) 0.0006(3) P3 0.0135(4) 0.0114(4) 0.0188(4) 0.0012(3) 0.0033(3) 0.0004(3) P4 0.0133(4) 0.0122(4) 0.0189(4) 0.0014(3) 0.0028(3) 0.0016(3) O1 0.0117(10) 0.0147(11) 0.0293(12) 0.0057(9) 0.0040(9) 0.0011(8) O2 0.0134(10) 0.0151(11) 0.0248(12) 0.0050(9) 0.0050(9) 0.0021(8) O3 0.0279(13) 0.0187(13) 0.0528(17) -0.0018(11) 0.0124(12) -0.0060(11) O4 0.0203(15) 0.0342(18) 0.151(4) 0.017(2) 0.0026(18) -0.0028(13) N1 0.0180(12) 0.0115(12) 0.0147(12) 0.0030(9) 0.0021(10) 0.0026(10) N2 0.0193(13) 0.0132(13) 0.0160(13) -0.0014(10) 0.0043(10) 0.0021(10) C1 0.0149(14) 0.0167(15) 0.0193(15) 0.0044(12) 0.0064(12) 0.0021(12) C2 0.0236(16) 0.0194(17) 0.0230(17) 0.0029(13) 0.0066(13) 0.0061(13) C3 0.0335(19) 0.0202(18) 0.036(2) 0.0070(15) 0.0162(16) 0.0127(15) C4 0.0298(19) 0.041(2) 0.0231(18) 0.0137(15) 0.0095(14) 0.0192(16) C5 0.0213(17) 0.041(2) 0.0222(17) 0.0052(15) 0.0041(13) 0.0008(15) C6 0.0203(16) 0.0240(18) 0.0237(17) 0.0038(13) 0.0030(13) 0.0010(13) C7 0.0282(17) 0.0096(15) 0.0195(16) 0.0009(12) -0.0016(13) 0.0010(12) C8 0.0278(18) 0.0179(17) 0.035(2) -0.0002(14) -0.0048(15) 0.0034(14) C9 0.046(2) 0.0200(19) 0.040(2) -0.0030(16) -0.0160(19) -0.0006(17) C10 0.065(3) 0.026(2) 0.025(2) -0.0006(15) -0.0092(19) 0.0001(19) C11 0.064(3) 0.030(2) 0.032(2) -0.0094(17) 0.017(2) -0.005(2) C12 0.038(2) 0.0255(19) 0.0244(18) -0.0060(14) 0.0087(15) -0.0070(16) C13 0.0154(14) 0.0166(16) 0.0229(16) 0.0042(12) 0.0035(12) -0.0010(12) C14 0.0229(17) 0.0200(17) 0.0350(19) 0.0104(14) 0.0091(14) 0.0033(14) C15 0.0283(18) 0.027(2) 0.043(2) 0.0160(16) 0.0132(16) 0.0014(15) C16 0.0228(17) 0.033(2) 0.042(2) 0.0091(17) 0.0179(16) 0.0027(15) C17 0.0203(16) 0.0231(18) 0.0329(19) 0.0036(14) 0.0089(14) 0.0021(14) C18 0.0174(15) 0.0133(15) 0.0245(16) 0.0044(12) 0.0040(12) -0.0017(12) C19 0.0118(13) 0.0226(17) 0.0244(17) 0.0018(13) 0.0032(12) 0.0031(13) C20 0.0197(15) 0.0164(15) 0.0151(15) 0.0000(11) 0.0041(12) 0.0017(12) C21 0.065(3) 0.0189(18) 0.0204(17) -0.0024(14) 0.0072(17) 0.0060(18) C22 0.0197(16) 0.038(2) 0.0180(16) 0.0034(14) 0.0004(13) -0.0012(15) C23 0.0214(17) 0.049(2) 0.0238(18) 0.0036(16) 0.0048(14) -0.0040(16) C24 0.0277(17) 0.0256(18) 0.0169(16) -0.0020(13) 0.0032(13) 0.0061(14) C25 0.067(3) 0.031(2) 0.0185(18) 0.0014(15) 0.0100(18) 0.013(2) C26 0.025(2) 0.093(4) 0.039(2) -0.035(2) 0.0003(17) -0.001(2) C27 0.039(2) 0.029(2) 0.0244(18) -0.0062(15) 0.0106(15) 0.0048(16) C28 0.0110(13) 0.0186(16) 0.0230(16) 0.0007(12) 0.0048(12) 0.0011(12) C29 0.0195(16) 0.0181(16) 0.0303(18) -0.0005(13) 0.0120(13) -0.0001(13) C30 0.0228(17) 0.0223(18) 0.0300(18) -0.0086(14) 0.0119(14) -0.0084(14) C31 0.0164(15) 0.034(2) 0.0234(17) -0.0045(14) 0.0052(13) -0.0047(14) C32 0.0160(15) 0.0205(17) 0.0249(17) 0.0008(13) 0.0050(12) 0.0003(12) C33 0.0140(14) 0.0131(15) 0.0225(16) -0.0027(12) 0.0065(12) -0.0010(11) C34 0.0138(14) 0.0154(15) 0.0232(16) 0.0029(12) 0.0008(12) -0.0002(12) C35 0.0259(17) 0.0271(19) 0.0250(18) 0.0041(14) 0.0090(14) 0.0060(14) C36 0.0288(18) 0.040(2) 0.0209(17) 0.0083(15) 0.0079(14) 0.0029(16) C37 0.0309(19) 0.030(2) 0.0272(19) 0.0110(15) -0.0019(15) 0.0016(16) C38 0.035(2) 0.0257(19) 0.0290(19) 0.0031(15) -0.0021(15) 0.0128(16) C39 0.0285(18) 0.0209(17) 0.0230(17) 0.0006(13) 0.0016(14) 0.0056(14) C40 0.0141(14) 0.0165(15) 0.0184(15) 0.0027(12) 0.0006(11) 0.0050(12) C41 0.0296(18) 0.0214(17) 0.0235(17) 0.0002(13) 0.0078(14) -0.0023(14) C42 0.038(2) 0.0197(17) 0.0256(18) -0.0039(14) 0.0047(15) 0.0007(15) C43 0.0312(19) 0.042(2) 0.0195(17) -0.0061(15) 0.0066(14) 0.0048(17) C44 0.031(2) 0.060(3) 0.038(2) -0.011(2) 0.0186(17) -0.012(2) C45 0.0277(19) 0.039(2) 0.0302(19) -0.0112(16) 0.0110(15) -0.0118(16) C46 0.0266(19) 0.0114(16) 0.063(3) 0.0070(16) 0.0059(18) -0.0007(14) C47 0.039(2) 0.035(2) 0.0284(19) -0.0003(16) 0.0125(16) -0.0039(17) Cl3 0.0651(8) 0.0671(9) 0.0676(8) 0.0300(7) 0.0330(7) 0.0227(7) Cl4 0.0783(9) 0.0836(10) 0.0600(8) 0.0277(7) 0.0461(7) 0.0383(8) _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 Rh1 C19 1.905(3) . ? Rh1 P2 2.1653(8) . ? Rh1 P1 2.3209(8) . ? Rh1 Cl1 2.3851(8) . ? Rh2 C46 1.889(4) . ? Rh2 P3 2.1665(8) . ? Rh2 P4 2.3275(8) . ? Rh2 Cl2 2.3647(8) . ? P1 C13 1.813(3) . ? P1 C1 1.815(3) . ? P1 C7 1.822(3) . ? P2 O1 1.638(2) . ? P2 N1 1.694(2) . ? P2 N2 1.699(3) . ? P3 O2 1.652(2) . ? P3 N2 1.686(3) . ? P3 N1 1.689(3) . ? P4 C33 1.814(3) . ? P4 C34 1.815(3) . ? P4 C40 1.815(3) . ? O1 C18 1.388(4) . ? O2 C28 1.392(3) . ? O3 C19 1.126(4) . ? O4 C46 1.119(4) . ? N1 C20 1.488(4) . ? N2 C24 1.495(4) . ? C1 C6 1.389(4) . ? C1 C2 1.397(4) . ? C2 C3 1.393(4) . ? C2 H2 0.9500 . ? C3 C4 1.377(5) . ? C3 H3 0.9500 . ? C4 C5 1.385(5) . ? C4 H4 0.9500 . ? C5 C6 1.386(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.388(4) . ? C7 C12 1.394(5) . ? C8 C9 1.391(5) . ? C8 H8 0.9500 . ? C9 C10 1.365(6) . ? C9 H9 0.9500 . ? C10 C11 1.380(6) . ? C10 H10 0.9500 . ? C11 C12 1.382(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.390(4) . ? C13 C14 1.410(4) . ? C14 C15 1.380(5) . ? C14 H14 0.9500 . ? C15 C16 1.382(5) . ? C15 H15 0.9500 . ? C16 C17 1.383(5) . ? C16 H16 0.9500 . ? C17 C18 1.394(4) . ? C17 H17 0.9500 . ? C20 C23 1.523(4) . ? C20 C21 1.523(4) . ? C20 C22 1.523(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.516(5) . ? C24 C27 1.524(5) . ? C24 C25 1.525(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.384(4) . ? C28 C33 1.395(4) . ? C29 C30 1.387(5) . ? C29 H29 0.9500 . ? C30 C31 1.389(5) . ? C30 H30 0.9500 . ? C31 C32 1.379(4) . ? C31 H31 0.9500 . ? C32 C33 1.394(4) . ? C32 H32 0.9500 . ? C34 C39 1.387(4) . ? C34 C35 1.388(4) . ? C35 C36 1.386(5) . ? C35 H35 0.9500 . ? C36 C37 1.381(5) . ? C36 H36 0.9500 . ? C37 C38 1.375(5) . ? C37 H37 0.9500 . ? C38 C39 1.391(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.383(5) . ? C40 C41 1.395(4) . ? C41 C42 1.381(5) . ? C41 H41 0.9500 . ? C42 C43 1.374(5) . ? C42 H42 0.9500 . ? C43 C44 1.370(5) . ? C43 H43 0.9500 . ? C44 C45 1.394(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C47 Cl4 1.733(4) . ? C47 Cl3 1.765(4) . ? C47 H47A 0.9900 . ? C47 H47B 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 C19 Rh1 P2 91.23(9) . . ? C19 Rh1 P1 173.72(10) . . ? P2 Rh1 P1 92.05(3) . . ? C19 Rh1 Cl1 89.57(9) . . ? P2 Rh1 Cl1 171.20(3) . . ? P1 Rh1 Cl1 88.01(3) . . ? C46 Rh2 P3 92.70(11) . . ? C46 Rh2 P4 175.95(11) . . ? P3 Rh2 P4 91.05(3) . . ? C46 Rh2 Cl2 88.35(11) . . ? P3 Rh2 Cl2 177.95(3) . . ? P4 Rh2 Cl2 87.85(3) . . ? C13 P1 C1 103.24(14) . . ? C13 P1 C7 105.50(15) . . ? C1 P1 C7 106.58(14) . . ? C13 P1 Rh1 116.14(11) . . ? C1 P1 Rh1 114.01(10) . . ? C7 P1 Rh1 110.54(11) . . ? O1 P2 N1 97.38(12) . . ? O1 P2 N2 106.45(12) . . ? N1 P2 N2 82.76(12) . . ? O1 P2 Rh1 116.53(8) . . ? N1 P2 Rh1 121.44(9) . . ? N2 P2 Rh1 125.01(9) . . ? O2 P3 N2 98.75(12) . . ? O2 P3 N1 105.46(12) . . ? N2 P3 N1 83.27(12) . . ? O2 P3 Rh2 113.94(8) . . ? N2 P3 Rh2 126.19(10) . . ? N1 P3 Rh2 123.41(9) . . ? C33 P4 C34 102.93(14) . . ? C33 P4 C40 105.17(14) . . ? C34 P4 C40 105.44(14) . . ? C33 P4 Rh2 115.58(10) . . ? C34 P4 Rh2 116.10(10) . . ? C40 P4 Rh2 110.53(10) . . ? C18 O1 P2 130.60(19) . . ? C28 O2 P3 123.29(19) . . ? C20 N1 P3 131.6(2) . . ? C20 N1 P2 130.8(2) . . ? P3 N1 P2 96.42(13) . . ? C24 N2 P3 131.9(2) . . ? C24 N2 P2 130.6(2) . . ? P3 N2 P2 96.32(13) . . ? C6 C1 C2 119.8(3) . . ? C6 C1 P1 118.0(2) . . ? C2 C1 P1 122.2(2) . . ? C3 C2 C1 119.5(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.3(3) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 119.9(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.1(3) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C8 C7 C12 119.3(3) . . ? C8 C7 P1 120.9(3) . . ? C12 C7 P1 119.6(3) . . ? C7 C8 C9 119.9(4) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 119.8(4) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 120.6(4) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C7 119.8(4) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C18 C13 C14 117.4(3) . . ? C18 C13 P1 120.9(2) . . ? C14 C13 P1 121.6(2) . . ? C15 C14 C13 121.6(3) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C16 119.5(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 120.5(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 119.7(3) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? O1 C18 C13 122.8(3) . . ? O1 C18 C17 115.7(3) . . ? C13 C18 C17 121.3(3) . . ? O3 C19 Rh1 175.6(3) . . ? N1 C20 C23 110.1(3) . . ? N1 C20 C21 107.9(2) . . ? C23 C20 C21 109.8(3) . . ? N1 C20 C22 108.7(2) . . ? C23 C20 C22 110.3(3) . . ? C21 C20 C22 110.1(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 C26 109.7(3) . . ? N2 C24 C27 108.6(3) . . ? C26 C24 C27 110.2(3) . . ? N2 C24 C25 108.5(3) . . ? C26 C24 C25 110.9(3) . . ? C27 C24 C25 108.9(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 O2 117.2(3) . . ? C29 C28 C33 121.5(3) . . ? O2 C28 C33 121.2(3) . . ? C28 C29 C30 119.3(3) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C29 C30 C31 120.1(3) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 120.1(3) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.9(3) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C32 C33 C28 118.0(3) . . ? C32 C33 P4 123.0(2) . . ? C28 C33 P4 119.0(2) . . ? C39 C34 C35 119.2(3) . . ? C39 C34 P4 122.4(2) . . ? C35 C34 P4 118.4(2) . . ? C36 C35 C34 120.5(3) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 119.8(3) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C38 C37 C36 120.3(3) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 120.1(3) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C34 C39 C38 120.2(3) . . ? C34 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C45 C40 C41 118.9(3) . . ? C45 C40 P4 122.6(3) . . ? C41 C40 P4 118.5(2) . . ? C42 C41 C40 120.1(3) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C43 C42 C41 120.8(3) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 119.6(3) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C45 120.4(4) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C40 C45 C44 120.2(3) . . ? C40 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? O4 C46 Rh2 175.7(3) . . ? Cl4 C47 Cl3 111.2(2) . . ? Cl4 C47 H47A 109.4 . . ? Cl3 C47 H47A 109.4 . . ? Cl4 C47 H47B 109.4 . . ? Cl3 C47 H47B 109.4 . . ? H47A C47 H47B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.833 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.107 #===END data_msb340a_0m _database_code_depnum_ccdc_archive 'CCDC 779803' #TrackingRef '- MSB-94.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44.5 H47 Cl5 N2 O2 P4 Pt2' _chemical_formula_sum 'C44.5 H47 Cl5 N2 O2 P4 Pt2' _chemical_formula_weight 1333.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 10.109(2) _cell_length_b 25.000(5) _cell_length_c 10.463(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.739(2) _cell_angle_gamma 90.00 _cell_volume 2504.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 9946 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.34 _exptl_crystal_description Parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1269 _exptl_absorpt_coefficient_mu 5.958 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5712 _exptl_absorpt_correction_T_max 0.7238 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 20 sec/frame. ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44127 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.36 _reflns_number_total 6370 _reflns_number_gt 5514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _publ_section_references ; Bruker-AXS (2009). APEX2, Version 2009.11-0, Madison, WI. Bruker-AXS (2009a). SAINT, Version 7.68A, Madison, WI Bruker-AXS (2008). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS and SHELXL. Acta Cryst. A64, 112-122. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. Spek, A. L. (2010). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands. ; _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. Because of the crystallographic mirror symmetry imposed on the molecule, the t-butyl groups are rotationally disordered across the mirror plane. Refinement of one orientation of each was performed subject to restraints making them approximate ideal geometry. The residual density at a site partially occupied by solvent dichloromethane whch was additionally disordered about the mirror was removed with the SQUEEZE option of PLATON (Spek, 2010). ; _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^)+(0.0599P)^2^+2.9153P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 6370 _refine_ls_number_parameters 295 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.079 _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 Pt1 Pt 0.730036(18) 0.629593(7) 0.942541(16) 0.02904(7) Uani 1 1 d . . . Cl1 Cl 0.8551(2) 0.68047(6) 1.12747(13) 0.0663(5) Uani 1 1 d . . . Cl2 Cl 0.73464(15) 0.55886(5) 1.08824(12) 0.0435(3) Uani 1 1 d . . . P1 P 0.69113(12) 0.70025(5) 0.81250(11) 0.0263(2) Uani 1 1 d . . . P2 P 0.62720(12) 0.57435(5) 0.77008(11) 0.0286(2) Uani 1 1 d . . . O1 O 0.6078(4) 0.68589(13) 0.6557(3) 0.0354(7) Uani 1 1 d . . . N1 N 0.5923(5) 0.7500 0.8400(5) 0.0280(10) Uani 1 2 d SD . . N2 N 0.8037(5) 0.7500 0.8108(5) 0.0285(11) Uani 1 2 d SD . . C1 C 0.6541(5) 0.6477(2) 0.5816(4) 0.0358(10) Uani 1 1 d . . . C2 C 0.6803(7) 0.6647(2) 0.4672(5) 0.0503(14) Uani 1 1 d . . . H2 H 0.6673 0.7008 0.4408 0.060 Uiso 1 1 calc R . . C3 C 0.7264(8) 0.6279(3) 0.3904(6) 0.0582(18) Uani 1 1 d . . . H3 H 0.7464 0.6394 0.3131 0.070 Uiso 1 1 calc R . . C4 C 0.7427(6) 0.5750(3) 0.4277(5) 0.0501(15) Uani 1 1 d . . . H4 H 0.7751 0.5503 0.3769 0.060 Uiso 1 1 calc R . . C5 C 0.7111(5) 0.5583(2) 0.5409(5) 0.0406(11) Uani 1 1 d . . . H5 H 0.7201 0.5220 0.5648 0.049 Uiso 1 1 calc R . . C6 C 0.6662(5) 0.59427(19) 0.6198(5) 0.0330(10) Uani 1 1 d . . . C7 C 0.6875(5) 0.5055(2) 0.7990(4) 0.0348(10) Uani 1 1 d . . . C8 C 0.8307(6) 0.4954(2) 0.8327(5) 0.0460(12) Uani 1 1 d . . . H8 H 0.8942 0.5239 0.8447 0.055 Uiso 1 1 calc R . . C9 C 0.8775(7) 0.4437(3) 0.8481(6) 0.0562(16) Uani 1 1 d . . . H9 H 0.9735 0.4367 0.8684 0.067 Uiso 1 1 calc R . . C10 C 0.7863(8) 0.4020(3) 0.8343(7) 0.0661(19) Uani 1 1 d . . . H10 H 0.8197 0.3667 0.8465 0.079 Uiso 1 1 calc R . . C11 C 0.6472(8) 0.4119(2) 0.8028(7) 0.0614(17) Uani 1 1 d . . . H11 H 0.5850 0.3831 0.7940 0.074 Uiso 1 1 calc R . . C12 C 0.5962(6) 0.4633(2) 0.7837(5) 0.0448(12) Uani 1 1 d . . . H12 H 0.4997 0.4696 0.7604 0.054 Uiso 1 1 calc R . . C13 C 0.4385(5) 0.57296(18) 0.7229(5) 0.0324(9) Uani 1 1 d . . . C14 C 0.3767(6) 0.5666(2) 0.8238(6) 0.0408(11) Uani 1 1 d . . . H14 H 0.4326 0.5620 0.9142 0.049 Uiso 1 1 calc R . . C15 C 0.2319(6) 0.5670(2) 0.7896(7) 0.0506(14) Uani 1 1 d . . . H15 H 0.1901 0.5620 0.8571 0.061 Uiso 1 1 calc R . . C16 C 0.1503(6) 0.5745(3) 0.6599(8) 0.0603(17) Uani 1 1 d . . . H16 H 0.0526 0.5753 0.6387 0.072 Uiso 1 1 calc R . . C17 C 0.2086(6) 0.5811(3) 0.5589(7) 0.0570(16) Uani 1 1 d . . . H17 H 0.1512 0.5862 0.4692 0.068 Uiso 1 1 calc R . . C18 C 0.3538(6) 0.5801(2) 0.5908(6) 0.0434(12) Uani 1 1 d . . . H18 H 0.3942 0.5843 0.5220 0.052 Uiso 1 1 calc R . . C19 C 0.9509(6) 0.7500 0.8091(6) 0.0382(16) Uani 1 2 d SD . . C20 C 1.0443(8) 0.7704(5) 0.9432(9) 0.068(5) Uani 0.50 1 d PD . . H20A H 1.0194 0.8070 0.9558 0.101 Uiso 0.50 1 calc PR . . H20B H 1.1408 0.7691 0.9450 0.101 Uiso 0.50 1 calc PR . . H20C H 1.0330 0.7482 1.0150 0.101 Uiso 1 2 calc SR . . C21 C 0.9891(11) 0.6920(3) 0.7885(14) 0.071(4) Uani 0.50 1 d PD . . H21A H 1.0116 0.6728 0.8735 0.107 Uiso 0.50 1 calc PR . . H21B H 1.0693 0.6916 0.7568 0.107 Uiso 0.50 1 calc PR . . H21C H 0.9106 0.6748 0.7223 0.107 Uiso 0.50 1 calc PR . . C22 C 0.9589(11) 0.7845(5) 0.6930(11) 0.078(5) Uani 0.50 1 d PD . . H22A H 0.9350 0.8211 0.7074 0.117 Uiso 0.50 1 calc PR . . H22B H 0.8939 0.7712 0.6093 0.117 Uiso 0.50 1 calc PR . . H22C H 1.0530 0.7834 0.6880 0.117 Uiso 0.50 1 calc PR . . C23 C 0.4603(7) 0.7500 0.8716(7) 0.050(2) Uani 1 2 d SD . . C24 C 0.4016(10) 0.6969(3) 0.8724(12) 0.053(3) Uani 0.50 1 d PDU . . H24A H 0.3789 0.6813 0.7831 0.079 Uiso 0.50 1 calc PR . . H24B H 0.3176 0.6995 0.8978 0.079 Uiso 0.50 1 calc PR . . H24C H 0.4694 0.6745 0.9369 0.079 Uiso 0.50 1 calc PR . . C25 C 0.4873(13) 0.7799(5) 1.0072(11) 0.091(5) Uani 0.50 1 d PDU . . H25A H 0.5501 0.7590 1.0796 0.137 Uiso 0.50 1 calc PR . . H25B H 0.3995 0.7851 1.0247 0.137 Uiso 0.50 1 calc PR . . H25C H 0.5292 0.8145 1.0024 0.137 Uiso 0.50 1 calc PR . . C26 C 0.3582(10) 0.7869(4) 0.7643(13) 0.076(4) Uani 0.50 1 d PDU . . H26A H 0.3368 0.7707 0.6757 0.115 Uiso 0.50 1 calc PR . . H26B H 0.4015 0.8215 0.7642 0.115 Uiso 0.50 1 calc PR . . H26C H 0.2726 0.7915 0.7862 0.115 Uiso 0.50 1 calc PR . . 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 Pt1 0.03629(11) 0.03010(11) 0.02082(10) 0.00083(6) 0.00930(7) -0.00374(7) Cl1 0.1053(13) 0.0562(9) 0.0247(6) 0.0014(6) 0.0033(7) -0.0384(9) Cl2 0.0681(8) 0.0355(6) 0.0284(6) 0.0049(5) 0.0176(6) -0.0043(6) P1 0.0314(5) 0.0283(5) 0.0205(5) -0.0003(4) 0.0101(4) -0.0015(4) P2 0.0332(6) 0.0285(6) 0.0252(5) -0.0021(4) 0.0110(5) -0.0010(5) O1 0.0469(19) 0.0347(17) 0.0222(15) -0.0028(13) 0.0076(14) -0.0007(15) N1 0.026(2) 0.036(3) 0.025(3) 0.000 0.013(2) 0.000 N2 0.029(3) 0.029(3) 0.032(3) 0.000 0.017(2) 0.000 C1 0.047(3) 0.038(2) 0.021(2) -0.0050(18) 0.0096(19) -0.008(2) C2 0.079(4) 0.046(3) 0.027(2) -0.002(2) 0.019(3) -0.017(3) C3 0.084(5) 0.071(4) 0.027(3) -0.015(3) 0.028(3) -0.023(3) C4 0.062(4) 0.064(4) 0.030(3) -0.016(2) 0.021(3) -0.009(3) C5 0.044(3) 0.047(3) 0.031(2) -0.011(2) 0.012(2) -0.004(2) C6 0.039(2) 0.037(2) 0.023(2) -0.0058(18) 0.0095(18) -0.0048(19) C7 0.044(3) 0.034(2) 0.026(2) 0.0008(18) 0.012(2) 0.005(2) C8 0.045(3) 0.050(3) 0.041(3) -0.003(2) 0.011(2) 0.002(2) C9 0.053(3) 0.062(4) 0.048(3) -0.001(3) 0.008(3) 0.025(3) C10 0.090(5) 0.042(3) 0.053(4) -0.002(3) 0.004(3) 0.025(3) C11 0.075(4) 0.033(3) 0.067(4) -0.004(3) 0.009(3) 0.004(3) C12 0.056(3) 0.034(3) 0.040(3) -0.003(2) 0.010(2) -0.001(2) C13 0.034(2) 0.027(2) 0.036(2) -0.0027(18) 0.0110(19) -0.0013(18) C14 0.045(3) 0.036(3) 0.045(3) 0.006(2) 0.019(2) 0.000(2) C15 0.046(3) 0.046(3) 0.067(4) 0.006(3) 0.029(3) 0.001(2) C16 0.034(3) 0.055(4) 0.089(5) -0.011(3) 0.017(3) 0.001(3) C17 0.039(3) 0.071(4) 0.051(4) -0.010(3) 0.001(3) 0.002(3) C18 0.041(3) 0.050(3) 0.038(3) -0.006(2) 0.009(2) -0.001(2) C19 0.026(3) 0.056(4) 0.039(4) 0.000 0.019(3) 0.000 C20 0.037(5) 0.118(15) 0.050(7) -0.029(7) 0.018(5) -0.017(6) C21 0.034(6) 0.076(10) 0.109(13) -0.024(9) 0.030(8) 0.007(6) C22 0.043(7) 0.115(13) 0.094(12) 0.036(10) 0.046(8) -0.006(7) C23 0.028(3) 0.078(6) 0.051(5) 0.000 0.021(3) 0.000 C24 0.035(5) 0.051(6) 0.086(7) 0.008(5) 0.037(5) -0.007(4) C25 0.086(7) 0.125(9) 0.095(8) -0.034(7) 0.074(7) -0.020(6) C26 0.055(6) 0.071(7) 0.110(9) 0.019(7) 0.035(6) 0.003(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 Pt1 P1 2.1869(12) . ? Pt1 P2 2.2447(12) . ? Pt1 Cl1 2.3212(14) . ? Pt1 Cl2 2.3253(12) . ? P1 O1 1.625(3) . ? P1 N1 1.677(3) . ? P1 N2 1.690(3) . ? P2 C6 1.810(5) . ? P2 C13 1.811(5) . ? P2 C7 1.818(5) . ? O1 C1 1.402(6) . ? N1 C23 1.474(7) . ? N1 P1 1.677(3) 4_575 ? N2 C19 1.494(7) . ? N2 P1 1.690(3) 4_575 ? C1 C2 1.374(7) . ? C1 C6 1.388(7) . ? C2 C3 1.395(9) . ? C2 H2 0.9400 . ? C3 C4 1.374(9) . ? C3 H3 0.9400 . ? C4 C5 1.386(7) . ? C4 H4 0.9400 . ? C5 C6 1.391(7) . ? C5 H5 0.9400 . ? C7 C12 1.377(7) . ? C7 C8 1.398(7) . ? C8 C9 1.369(8) . ? C8 H8 0.9400 . ? C9 C10 1.368(10) . ? C9 H9 0.9400 . ? C10 C11 1.360(10) . ? C10 H10 0.9400 . ? C11 C12 1.376(8) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C18 1.384(7) . ? C13 C14 1.398(7) . ? C14 C15 1.391(7) . ? C14 H14 0.9400 . ? C15 C16 1.357(9) . ? C15 H15 0.9400 . ? C16 C17 1.374(10) . ? C16 H16 0.9400 . ? C17 C18 1.397(8) . ? C17 H17 0.9400 . ? C18 H18 0.9400 . ? C19 C20 1.506(7) . ? C19 C22 1.513(7) . ? C19 C21 1.534(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 C24 1.455(6) . ? C23 C25 1.549(7) . ? C23 C26 1.560(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 93.01(4) . . ? P1 Pt1 Cl1 90.97(5) . . ? P2 Pt1 Cl1 174.13(6) . . ? P1 Pt1 Cl2 169.68(5) . . ? P2 Pt1 Cl2 88.04(5) . . ? Cl1 Pt1 Cl2 88.82(5) . . ? O1 P1 N1 101.1(2) . . ? O1 P1 N2 106.5(2) . . ? N1 P1 N2 84.05(16) . . ? O1 P1 Pt1 112.38(13) . . ? N1 P1 Pt1 119.35(15) . . ? N2 P1 Pt1 127.88(17) . . ? C6 P2 C13 105.8(2) . . ? C6 P2 C7 104.5(2) . . ? C13 P2 C7 107.1(2) . . ? C6 P2 Pt1 110.82(16) . . ? C13 P2 Pt1 113.97(15) . . ? C7 P2 Pt1 113.87(16) . . ? C1 O1 P1 123.5(3) . . ? C23 N1 P1 132.11(12) . 4_575 ? C23 N1 P1 132.11(12) . . ? P1 N1 P1 95.7(2) 4_575 . ? C19 N2 P1 132.60(12) . . ? C19 N2 P1 132.60(12) . 4_575 ? P1 N2 P1 94.8(2) . 4_575 ? C2 C1 C6 121.7(5) . . ? C2 C1 O1 117.6(5) . . ? C6 C1 O1 120.7(4) . . ? C1 C2 C3 119.4(6) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 120.2(5) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.5(5) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 121.4(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 117.8(4) . . ? C1 C6 P2 119.4(3) . . ? C5 C6 P2 122.8(4) . . ? C12 C7 C8 119.4(5) . . ? C12 C7 P2 122.0(4) . . ? C8 C7 P2 118.5(4) . . ? C9 C8 C7 119.4(6) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 120.7(6) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 119.8(6) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 121.0(6) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C7 119.6(6) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C18 C13 C14 119.1(5) . . ? C18 C13 P2 122.0(4) . . ? C14 C13 P2 118.9(4) . . ? C15 C14 C13 119.6(5) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C16 C15 C14 120.7(6) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 120.8(6) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C18 119.5(6) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 120.4(6) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? N2 C19 C20 108.5(5) . . ? N2 C19 C22 108.7(5) . . ? C20 C19 C22 112.1(6) . . ? N2 C19 C21 107.4(5) . . ? C20 C19 C21 109.8(6) . . ? C22 C19 C21 110.2(6) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 N1 113.6(4) . . ? C24 C23 C25 112.8(7) . . ? N1 C23 C25 107.4(5) . . ? C24 C23 C26 111.6(7) . . ? N1 C23 C26 106.0(5) . . ? C25 C23 C26 104.8(6) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.829 _refine_diff_density_min -1.849 _refine_diff_density_rms 0.162 # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.205 0.750 0.372 133 38 ' ' 2 -0.205 0.250 0.628 133 38 ' ' _platon_squeeze_details ; A region of density about the mirror plane was tentatively identified as lattice dichloromethane on the basis of trial refinements but the site was clearly only partially occupied and the lattice molecule was additionally disordered about the mirror. Following several unsuccessful attempts to model this region of density, it was decided to remove it. ; #===END data_14b _database_code_depnum_ccdc_archive 'CCDC 779804' #TrackingRef '- MSB-94.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C44 H46 Cl2 N2 O3 P4 Pd2), C3 H5 Cl Pd' _chemical_formula_sum 'C91 H97 Cl5 N4 O6 P8 Pd5' _chemical_formula_weight 2299.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9307(6) _cell_length_b 14.9928(8) _cell_length_c 16.6719(8) _cell_angle_alpha 115.282(1) _cell_angle_beta 92.342(1) _cell_angle_gamma 99.743(1) _cell_volume 2415.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9513 _cell_measurement_theta_min 2.335 _cell_measurement_theta_max 27.691 _exptl_crystal_description Column _exptl_crystal_colour 'Clear yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1154 _exptl_absorpt_coefficient_mu 1.236 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7544 _exptl_absorpt_correction_T_max 0.9044 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41376 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.71 _reflns_number_total 11233 _reflns_number_gt 9104 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2006)' _publ_section_references ; Bruker-AXS (2006). APEX2, Version 2.1-0, Madison, WI. Bruker-AXS (2006a). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2004). SADABS, Version 2004/2. University of G\"ottingen, Germany. ; _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. The [(\h^3^-C~3~H~5~)Pd(\m-Cl)]~2~ unit has crystallographically-imposed centrosymmetry and, on the basis of trial refinements of occupancy parameters, an occupancy of 0.5. In addition, the allyl ligand is disordered over two approximately equally occupied sites. The final refinement was performed with these occupancy restraints as well as those restraining the two orientations of the allyl group to have idealized geometry. The largest peak in the final difference map is approximately 1.25 \%A from the metal atom of the allylpalladium chloride moiety and thus is not in a chemically reasonable position to be part of this unit. It may be part of a solvent molecule also partially occupying this site but no chemically reasonable model for it could be devised. ; _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^)+(0.0740P)^2^+9.4078P] 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 11233 _refine_ls_number_parameters 571 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1483 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.054 _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 Pd1 Pd 0.14717(3) 0.06061(3) 0.24366(2) 0.01948(10) Uani 1 1 d . . . Pd2 Pd 0.02970(3) 0.23379(3) 0.49634(2) 0.01986(10) Uani 1 1 d . . . Cl1 Cl -0.01996(10) -0.02067(9) 0.12772(8) 0.0264(2) Uani 1 1 d . . . Cl2 Cl -0.00539(10) 0.10069(9) 0.34689(8) 0.0269(2) Uani 1 1 d . . . P1 P 0.28316(11) 0.02873(9) 0.14423(8) 0.0218(2) Uani 1 1 d . . . P2 P 0.29714(11) 0.14473(9) 0.35778(8) 0.0212(2) Uani 1 1 d . . . P3 P 0.23647(11) 0.24286(9) 0.50929(8) 0.0242(3) Uani 1 1 d . . . P4 P 0.03255(11) 0.35386(9) 0.63346(8) 0.0226(2) Uani 1 1 d . . . O1 O 0.4404(3) 0.1462(3) 0.3386(2) 0.0274(7) Uani 1 1 d . . . O2 O -0.1619(3) 0.2304(3) 0.4833(2) 0.0265(7) Uani 1 1 d . . . O3 O 0.3115(3) 0.3025(3) 0.5980(2) 0.0347(9) Uani 1 1 d . . . N1 N 0.2766(4) 0.1276(3) 0.4482(3) 0.0244(8) Uani 1 1 d . . . N2 N 0.2914(4) 0.2640(3) 0.4211(3) 0.0247(8) Uani 1 1 d . . . C1 C 0.3090(5) 0.1282(4) 0.1084(3) 0.0262(10) Uani 1 1 d . . . C2 C 0.2035(5) 0.1637(4) 0.0909(3) 0.0291(10) Uani 1 1 d . . . H2 H 0.1219 0.1335 0.0954 0.035 Uiso 1 1 calc R . . C3 C 0.2199(6) 0.2428(4) 0.0672(4) 0.0363(12) Uani 1 1 d . . . H3 H 0.1494 0.2668 0.0555 0.044 Uiso 1 1 calc R . . C4 C 0.3391(6) 0.2871(4) 0.0606(4) 0.0365(12) Uani 1 1 d . . . H4 H 0.3497 0.3410 0.0442 0.044 Uiso 1 1 calc R . . C5 C 0.4429(5) 0.2526(4) 0.0778(3) 0.0346(12) Uani 1 1 d . . . H5 H 0.5242 0.2827 0.0728 0.042 Uiso 1 1 calc R . . C6 C 0.4277(5) 0.1739(4) 0.1025(3) 0.0290(10) Uani 1 1 d . . . H6 H 0.4988 0.1514 0.1153 0.035 Uiso 1 1 calc R . . C7 C 0.2290(4) -0.0904(4) 0.0462(3) 0.0258(10) Uani 1 1 d . . . C8 C 0.1995(5) -0.0934(4) -0.0368(3) 0.0314(11) Uani 1 1 d . . . H8 H 0.2105 -0.0327 -0.0434 0.038 Uiso 1 1 calc R . . C9 C 0.1538(6) -0.1861(4) -0.1106(4) 0.0399(13) Uani 1 1 d . . . H9 H 0.1321 -0.1885 -0.1674 0.048 Uiso 1 1 calc R . . C10 C 0.1399(6) -0.2743(4) -0.1013(4) 0.0419(14) Uani 1 1 d . . . H10 H 0.1102 -0.3375 -0.1517 0.050 Uiso 1 1 calc R . . C11 C 0.1694(6) -0.2705(4) -0.0179(4) 0.0444(14) Uani 1 1 d . . . H11 H 0.1593 -0.3313 -0.0116 0.053 Uiso 1 1 calc R . . C12 C 0.2135(6) -0.1787(4) 0.0563(4) 0.0365(12) Uani 1 1 d . . . H12 H 0.2328 -0.1764 0.1134 0.044 Uiso 1 1 calc R . . C13 C 0.4369(4) 0.0220(4) 0.1833(3) 0.0229(9) Uani 1 1 d . . . C14 C 0.5053(4) -0.0401(4) 0.1207(3) 0.0295(11) Uani 1 1 d . . . H14 H 0.4682 -0.0794 0.0604 0.035 Uiso 1 1 calc R . . C15 C 0.6255(5) -0.0449(4) 0.1453(4) 0.0329(12) Uani 1 1 d . . . H15 H 0.6705 -0.0868 0.1021 0.039 Uiso 1 1 calc R . . C16 C 0.6800(4) 0.0122(4) 0.2337(3) 0.0299(11) Uani 1 1 d . . . H16 H 0.7626 0.0091 0.2507 0.036 Uiso 1 1 calc R . . C17 C 0.6149(4) 0.0736(4) 0.2972(3) 0.0254(10) Uani 1 1 d . . . H17 H 0.6520 0.1119 0.3576 0.030 Uiso 1 1 calc R . . C18 C 0.4942(4) 0.0780(3) 0.2709(3) 0.0217(9) Uani 1 1 d . . . C19 C 0.2780(5) 0.0404(4) 0.4678(4) 0.0315(11) Uani 1 1 d . . . C20 C 0.3005(6) -0.0469(4) 0.3848(4) 0.0386(13) Uani 1 1 d . . . H20A H 0.2369 -0.0617 0.3352 0.058 Uiso 1 1 calc R . . H20B H 0.2955 -0.1064 0.3960 0.058 Uiso 1 1 calc R . . H20C H 0.3837 -0.0294 0.3692 0.058 Uiso 1 1 calc R . . C21 C 0.3822(8) 0.0724(6) 0.5440(5) 0.0586(19) Uani 1 1 d . . . H21A H 0.4617 0.0961 0.5272 0.088 Uiso 1 1 calc R . . H21B H 0.3886 0.0147 0.5560 0.088 Uiso 1 1 calc R . . H21C H 0.3633 0.1268 0.5978 0.088 Uiso 1 1 calc R . . C22 C 0.1563(7) 0.0122(5) 0.4974(6) 0.0573(19) Uani 1 1 d . . . H22A H 0.1455 0.0680 0.5533 0.086 Uiso 1 1 calc R . . H22B H 0.1562 -0.0479 0.5070 0.086 Uiso 1 1 calc R . . H22C H 0.0876 -0.0022 0.4513 0.086 Uiso 1 1 calc R . . C23 C -0.1294(5) 0.3644(4) 0.6311(3) 0.0260(10) Uani 1 1 d . . . C24 C -0.2048(4) 0.2953(4) 0.5514(3) 0.0266(10) Uani 1 1 d . . . C25 C -0.3345(5) 0.2984(4) 0.5473(4) 0.0310(11) Uani 1 1 d . . . H25 H -0.3894 0.2540 0.4943 0.037 Uiso 1 1 calc R . . C26 C -0.3813(5) 0.3656(4) 0.6200(4) 0.0343(12) Uani 1 1 d . . . H26 H -0.4682 0.3657 0.6161 0.041 Uiso 1 1 calc R . . C27 C -0.3038(5) 0.4331(4) 0.6988(4) 0.0342(12) Uani 1 1 d . . . H27 H -0.3373 0.4785 0.7480 0.041 Uiso 1 1 calc R . . C28 C -0.1779(5) 0.4326(4) 0.7038(4) 0.0330(11) Uani 1 1 d . . . H28 H -0.1237 0.4785 0.7567 0.040 Uiso 1 1 calc R . . C29 C 0.1271(4) 0.4778(3) 0.6638(3) 0.0248(10) Uani 1 1 d . . . C30 C 0.0848(5) 0.5396(4) 0.6311(4) 0.0303(11) Uani 1 1 d . . . H30 H 0.0034 0.5193 0.5988 0.036 Uiso 1 1 calc R . . C31 C 0.1599(5) 0.6308(4) 0.6449(4) 0.0375(13) Uani 1 1 d . . . H31 H 0.1313 0.6722 0.6213 0.045 Uiso 1 1 calc R . . C32 C 0.2790(5) 0.6605(4) 0.6946(4) 0.0379(13) Uani 1 1 d . . . H32 H 0.3310 0.7231 0.7054 0.045 Uiso 1 1 calc R . . C33 C 0.3202(5) 0.6007(4) 0.7272(4) 0.0373(13) Uani 1 1 d . . . H33 H 0.4008 0.6218 0.7608 0.045 Uiso 1 1 calc R . . C34 C 0.2456(5) 0.5082(4) 0.7120(3) 0.0290(10) Uani 1 1 d . . . H34 H 0.2757 0.4663 0.7344 0.035 Uiso 1 1 calc R . . C35 C 0.0613(5) 0.3207(4) 0.7238(4) 0.0319(11) Uani 1 1 d . . . C36 C 0.0806(6) 0.3927(5) 0.8135(4) 0.0425(14) Uani 1 1 d . . . H36 H 0.0892 0.4622 0.8282 0.051 Uiso 1 1 calc R . . C37 C 0.0872(8) 0.3614(6) 0.8810(5) 0.0561(18) Uani 1 1 d . . . H37 H 0.1006 0.4094 0.9421 0.067 Uiso 1 1 calc R . . C38 C 0.0740(8) 0.2591(6) 0.8579(5) 0.060(2) Uani 1 1 d . . . H38 H 0.0787 0.2376 0.9038 0.072 Uiso 1 1 calc R . . C39 C 0.0546(8) 0.1896(5) 0.7712(5) 0.0577(19) Uani 1 1 d . . . H39 H 0.0462 0.1201 0.7565 0.069 Uiso 1 1 calc R . . C40 C 0.0471(6) 0.2204(5) 0.7036(4) 0.0431(14) Uani 1 1 d . . . H40 H 0.0319 0.1715 0.6428 0.052 Uiso 1 1 calc R . . C41 C 0.2889(5) 0.3481(4) 0.3968(4) 0.0323(12) Uani 1 1 d . . . C42 C 0.1639(6) 0.3294(6) 0.3396(6) 0.060(2) Uani 1 1 d . . . H42A H 0.1534 0.2655 0.2856 0.090 Uiso 1 1 calc R . . H42B H 0.1647 0.3846 0.3227 0.090 Uiso 1 1 calc R . . H42C H 0.0945 0.3264 0.3743 0.090 Uiso 1 1 calc R . . C43 C 0.3950(5) 0.3517(4) 0.3403(4) 0.0365(12) Uani 1 1 d . . . H43A H 0.4752 0.3621 0.3749 0.055 Uiso 1 1 calc R . . H43B H 0.3958 0.4073 0.3241 0.055 Uiso 1 1 calc R . . H43C H 0.3820 0.2879 0.2859 0.055 Uiso 1 1 calc R . . C44 C 0.3101(9) 0.4442(5) 0.4835(5) 0.063(2) Uani 1 1 d . . . H44A H 0.2415 0.4407 0.5188 0.095 Uiso 1 1 calc R . . H44B H 0.3129 0.5020 0.4701 0.095 Uiso 1 1 calc R . . H44C H 0.3896 0.4519 0.5176 0.095 Uiso 1 1 calc R . . Pd3 Pd 0.48512(7) 0.39089(6) 0.90278(5) 0.02616(17) Uani 0.50 1 d PD . . Cl3 Cl 0.3712(3) 0.5232(3) 0.9621(3) 0.0649(12) Uani 0.50 1 d P . . C45 C 0.5595(8) 0.2541(8) 0.8096(9) 0.037(3) Uani 0.25 1 d PD A 1 H45A H 0.5423 0.2333 0.8551 0.045 Uiso 0.25 1 calc PR A 1 H45B H 0.6406 0.2571 0.7912 0.045 Uiso 0.25 1 calc PR A 1 C46 C 0.4759(14) 0.2774(15) 0.7741(13) 0.043(4) Uani 0.25 1 d PDU A 1 H46 H 0.4967 0.2978 0.7289 0.052 Uiso 0.25 1 calc PR A 1 C47 C 0.3670(14) 0.2760(13) 0.7935(11) 0.026(3) Uani 0.25 1 d PDU A 1 H47A H 0.3428 0.2559 0.8384 0.031 Uiso 0.25 1 calc PR A 1 H47B H 0.3082 0.2948 0.7634 0.031 Uiso 0.25 1 calc PR A 1 C45A C 0.5595(8) 0.2541(8) 0.8096(9) 0.037(3) Uani 0.25 1 d PD A 2 H45C H 0.6120 0.3007 0.7947 0.045 Uiso 0.25 1 calc PR A 2 H45D H 0.5950 0.2118 0.8289 0.045 Uiso 0.25 1 calc PR A 2 C46A C 0.4408(15) 0.2484(14) 0.8038(14) 0.043(4) Uani 0.25 1 d PDU A 2 H46A H 0.3858 0.2026 0.8182 0.052 Uiso 0.25 1 calc PR A 2 C47A C 0.4006(17) 0.3089(13) 0.7769(10) 0.026(3) Uani 0.25 1 d PDU A 2 H47C H 0.4581 0.3538 0.7630 0.031 Uiso 0.25 1 calc PR A 2 H47D H 0.3136 0.3084 0.7712 0.031 Uiso 0.25 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01518(16) 0.02288(18) 0.02016(18) 0.00898(14) 0.00128(12) 0.00500(12) Pd2 0.01645(17) 0.02098(17) 0.02076(18) 0.00786(13) 0.00298(13) 0.00387(12) Cl1 0.0193(5) 0.0347(6) 0.0239(6) 0.0119(5) -0.0014(4) 0.0057(4) Cl2 0.0160(5) 0.0308(6) 0.0240(6) 0.0038(4) 0.0023(4) 0.0025(4) P1 0.0178(5) 0.0261(6) 0.0208(6) 0.0095(5) 0.0016(4) 0.0055(4) P2 0.0162(5) 0.0222(6) 0.0218(6) 0.0060(4) 0.0025(4) 0.0051(4) P3 0.0177(5) 0.0260(6) 0.0226(6) 0.0047(5) 0.0020(4) 0.0053(4) P4 0.0206(5) 0.0232(6) 0.0219(6) 0.0084(5) 0.0038(4) 0.0031(4) O1 0.0157(15) 0.0289(18) 0.0256(18) 0.0009(14) 0.0039(13) 0.0041(13) O2 0.0200(16) 0.0297(18) 0.0240(17) 0.0067(14) 0.0017(13) 0.0049(13) O3 0.0258(18) 0.039(2) 0.0269(19) 0.0025(16) 0.0000(15) 0.0101(15) N1 0.0235(19) 0.027(2) 0.022(2) 0.0083(16) 0.0025(15) 0.0093(15) N2 0.0189(18) 0.0222(19) 0.028(2) 0.0060(16) 0.0094(16) 0.0050(15) C1 0.028(2) 0.028(2) 0.020(2) 0.0084(19) 0.0027(19) 0.0055(19) C2 0.028(2) 0.033(3) 0.027(3) 0.014(2) 0.002(2) 0.007(2) C3 0.044(3) 0.037(3) 0.034(3) 0.021(2) 0.002(2) 0.013(2) C4 0.052(3) 0.029(3) 0.028(3) 0.014(2) 0.003(2) 0.005(2) C5 0.039(3) 0.032(3) 0.025(3) 0.009(2) 0.005(2) -0.003(2) C6 0.028(2) 0.035(3) 0.022(2) 0.011(2) 0.0043(19) 0.004(2) C7 0.020(2) 0.030(2) 0.021(2) 0.0041(19) 0.0020(18) 0.0074(18) C8 0.033(3) 0.034(3) 0.026(3) 0.011(2) -0.001(2) 0.011(2) C9 0.043(3) 0.041(3) 0.027(3) 0.005(2) 0.000(2) 0.014(3) C10 0.036(3) 0.034(3) 0.039(3) 0.001(2) 0.005(2) 0.007(2) C11 0.053(4) 0.030(3) 0.046(4) 0.012(3) 0.010(3) 0.008(3) C12 0.048(3) 0.027(3) 0.034(3) 0.013(2) 0.000(2) 0.007(2) C13 0.019(2) 0.027(2) 0.023(2) 0.0104(19) 0.0020(17) 0.0051(17) C14 0.021(2) 0.039(3) 0.022(2) 0.008(2) 0.0007(19) 0.009(2) C15 0.020(2) 0.041(3) 0.030(3) 0.006(2) 0.007(2) 0.012(2) C16 0.016(2) 0.035(3) 0.030(3) 0.007(2) 0.0003(19) 0.0065(19) C17 0.018(2) 0.028(2) 0.025(2) 0.0069(19) 0.0000(18) 0.0046(17) C18 0.021(2) 0.022(2) 0.020(2) 0.0066(17) 0.0038(17) 0.0056(17) C19 0.033(3) 0.036(3) 0.033(3) 0.019(2) 0.008(2) 0.014(2) C20 0.052(4) 0.032(3) 0.035(3) 0.015(2) 0.008(3) 0.018(2) C21 0.075(5) 0.056(4) 0.046(4) 0.022(3) -0.011(4) 0.022(4) C22 0.056(4) 0.049(4) 0.086(6) 0.040(4) 0.038(4) 0.024(3) C23 0.023(2) 0.029(2) 0.024(2) 0.0104(19) 0.0053(18) 0.0048(18) C24 0.024(2) 0.028(2) 0.030(3) 0.015(2) 0.0037(19) 0.0047(18) C25 0.021(2) 0.036(3) 0.032(3) 0.013(2) 0.005(2) 0.003(2) C26 0.024(2) 0.039(3) 0.038(3) 0.015(2) 0.009(2) 0.007(2) C27 0.031(3) 0.033(3) 0.036(3) 0.010(2) 0.016(2) 0.013(2) C28 0.030(3) 0.033(3) 0.030(3) 0.009(2) 0.008(2) 0.004(2) C29 0.025(2) 0.022(2) 0.025(2) 0.0080(18) 0.0075(19) 0.0037(17) C30 0.028(2) 0.029(3) 0.034(3) 0.013(2) 0.007(2) 0.009(2) C31 0.040(3) 0.033(3) 0.047(3) 0.022(3) 0.019(3) 0.011(2) C32 0.033(3) 0.029(3) 0.048(3) 0.012(2) 0.019(3) 0.006(2) C33 0.029(3) 0.034(3) 0.035(3) 0.005(2) 0.009(2) 0.000(2) C34 0.026(2) 0.029(2) 0.028(3) 0.009(2) 0.007(2) 0.0052(19) C35 0.033(3) 0.036(3) 0.028(3) 0.017(2) 0.003(2) 0.002(2) C36 0.055(4) 0.040(3) 0.031(3) 0.015(2) 0.008(3) 0.010(3) C37 0.075(5) 0.061(4) 0.033(3) 0.022(3) 0.007(3) 0.012(4) C38 0.093(6) 0.051(4) 0.039(4) 0.025(3) 0.002(4) 0.010(4) C39 0.097(6) 0.035(3) 0.045(4) 0.023(3) 0.009(4) 0.011(3) C40 0.059(4) 0.036(3) 0.037(3) 0.019(3) 0.004(3) 0.008(3) C41 0.029(3) 0.023(2) 0.045(3) 0.012(2) 0.018(2) 0.0082(19) C42 0.035(3) 0.060(4) 0.115(7) 0.065(5) 0.012(4) 0.013(3) C43 0.035(3) 0.036(3) 0.039(3) 0.016(2) 0.018(2) 0.007(2) C44 0.109(6) 0.026(3) 0.055(4) 0.013(3) 0.054(4) 0.015(3) Pd3 0.0215(3) 0.0252(4) 0.0315(4) 0.0158(3) -0.0071(3) -0.0021(3) Cl3 0.0458(18) 0.0491(18) 0.067(2) -0.0048(16) -0.0364(17) 0.0201(14) C45 0.014(4) 0.028(5) 0.091(9) 0.046(6) 0.005(5) 0.004(4) C46 0.046(5) 0.040(5) 0.040(5) 0.017(3) 0.009(3) 0.002(3) C47 0.027(4) 0.028(4) 0.023(4) 0.012(3) 0.005(3) 0.004(3) C45A 0.014(4) 0.028(5) 0.091(9) 0.046(6) 0.005(5) 0.004(4) C46A 0.046(5) 0.040(5) 0.040(5) 0.017(3) 0.009(3) 0.002(3) C47A 0.027(4) 0.028(4) 0.023(4) 0.012(3) 0.005(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P2 2.2121(12) . ? Pd1 P1 2.2252(12) . ? Pd1 Cl1 2.3462(11) . ? Pd1 Cl2 2.4071(12) . ? Pd2 O2 2.087(3) . ? Pd2 P4 2.2199(13) . ? Pd2 P3 2.2371(12) . ? Pd2 Cl2 2.3987(12) . ? P1 C13 1.811(5) . ? P1 C7 1.811(5) . ? P1 C1 1.815(5) . ? P2 O1 1.610(3) . ? P2 N1 1.652(4) . ? P2 N2 1.657(4) . ? P3 O3 1.477(4) . ? P3 N1 1.734(4) . ? P3 N2 1.740(4) . ? P4 C23 1.804(5) . ? P4 C35 1.808(5) . ? P4 C29 1.811(5) . ? O1 C18 1.391(5) . ? O2 C24 1.307(6) . ? N1 C19 1.478(6) . ? N2 C41 1.484(7) . ? C1 C6 1.389(7) . ? C1 C2 1.417(7) . ? C2 C3 1.389(7) . ? C2 H2 0.9500 . ? C3 C4 1.390(8) . ? C3 H3 0.9500 . ? C4 C5 1.392(8) . ? C4 H4 0.9500 . ? C5 C6 1.394(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.388(7) . ? C7 C8 1.389(7) . ? C8 C9 1.397(7) . ? C8 H8 0.9500 . ? C9 C10 1.381(9) . ? C9 H9 0.9500 . ? C10 C11 1.388(9) . ? C10 H10 0.9500 . ? C11 C12 1.390(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.390(6) . ? C13 C14 1.409(7) . ? C14 C15 1.383(7) . ? C14 H14 0.9500 . ? C15 C16 1.392(7) . ? C15 H15 0.9500 . ? C16 C17 1.387(7) . ? C16 H16 0.9500 . ? C17 C18 1.395(6) . ? C17 H17 0.9500 . ? C19 C22 1.494(8) . ? C19 C20 1.511(8) . ? C19 C21 1.522(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.401(7) . ? C23 C28 1.405(7) . ? C24 C25 1.426(7) . ? C25 C26 1.389(8) . ? C25 H25 0.9500 . ? C26 C27 1.397(8) . ? C26 H26 0.9500 . ? C27 C28 1.376(8) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.388(7) . ? C29 C34 1.391(7) . ? C30 C31 1.390(7) . ? C30 H30 0.9500 . ? C31 C32 1.407(9) . ? C31 H31 0.9500 . ? C32 C33 1.356(9) . ? C32 H32 0.9500 . ? C33 C34 1.397(7) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.372(8) . ? C35 C36 1.401(8) . ? C36 C37 1.396(9) . ? C36 H36 0.9500 . ? C37 C38 1.392(10) . ? C37 H37 0.9500 . ? C38 C39 1.354(10) . ? C38 H38 0.9500 . ? C39 C40 1.393(9) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C44 1.516(8) . ? C41 C43 1.532(7) . ? C41 C42 1.546(9) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? Pd3 C47A 2.005(15) . ? Pd3 C46A 2.024(19) . ? Pd3 C46 2.077(19) . ? Pd3 C47 2.080(15) . ? Pd3 C45 2.286(12) . ? Pd3 Cl3 2.393(3) . ? Pd3 Cl3 2.397(3) 2_667 ? Cl3 Pd3 2.397(3) 2_667 ? C45 C46 1.244(15) . ? C45 H45A 0.9500 . ? C45 H45B 0.9500 . ? C46 C47 1.245(16) . ? C46 H46 0.9500 . ? C47 H47A 0.9500 . ? C47 H47B 0.9500 . ? C46A C47A 1.298(16) . ? C46A H46A 0.9500 . ? C47A H47C 0.9500 . ? C47A H47D 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 Pd1 P1 92.65(4) . . ? P2 Pd1 Cl1 176.16(4) . . ? P1 Pd1 Cl1 90.37(4) . . ? P2 Pd1 Cl2 89.07(4) . . ? P1 Pd1 Cl2 176.44(5) . . ? Cl1 Pd1 Cl2 87.79(4) . . ? O2 Pd2 P4 85.07(10) . . ? O2 Pd2 P3 177.71(11) . . ? P4 Pd2 P3 94.51(5) . . ? O2 Pd2 Cl2 86.81(10) . . ? P4 Pd2 Cl2 171.79(4) . . ? P3 Pd2 Cl2 93.66(4) . . ? Pd2 Cl2 Pd1 126.18(5) . . ? C13 P1 C7 104.6(2) . . ? C13 P1 C1 105.7(2) . . ? C7 P1 C1 108.3(2) . . ? C13 P1 Pd1 115.95(16) . . ? C7 P1 Pd1 112.53(16) . . ? C1 P1 Pd1 109.28(17) . . ? O1 P2 N1 110.2(2) . . ? O1 P2 N2 105.32(19) . . ? N1 P2 N2 86.0(2) . . ? O1 P2 Pd1 118.51(13) . . ? N1 P2 Pd1 116.13(15) . . ? N2 P2 Pd1 115.73(15) . . ? O3 P3 N1 113.7(2) . . ? O3 P3 N2 116.8(2) . . ? N1 P3 N2 81.0(2) . . ? O3 P3 Pd2 119.37(16) . . ? N1 P3 Pd2 112.70(14) . . ? N2 P3 Pd2 106.94(14) . . ? C23 P4 C35 105.1(2) . . ? C23 P4 C29 107.7(2) . . ? C35 P4 C29 107.9(2) . . ? C23 P4 Pd2 100.34(17) . . ? C35 P4 Pd2 116.04(19) . . ? C29 P4 Pd2 118.34(16) . . ? C18 O1 P2 131.3(3) . . ? C24 O2 Pd2 116.9(3) . . ? C19 N1 P2 132.7(3) . . ? C19 N1 P3 131.6(3) . . ? P2 N1 P3 95.4(2) . . ? C41 N2 P2 130.3(4) . . ? C41 N2 P3 131.4(3) . . ? P2 N2 P3 95.0(2) . . ? C6 C1 C2 119.5(5) . . ? C6 C1 P1 122.5(4) . . ? C2 C1 P1 117.9(4) . . ? C3 C2 C1 119.6(5) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 120.3(5) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 120.2(5) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.0(5) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 120.4(5) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C12 C7 C8 120.6(5) . . ? C12 C7 P1 118.6(4) . . ? C8 C7 P1 120.8(4) . . ? C7 C8 C9 119.6(5) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 120.1(6) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.8(5) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 120.7(6) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C7 C12 C11 119.2(5) . . ? C7 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C18 C13 C14 117.7(4) . . ? C18 C13 P1 123.8(4) . . ? C14 C13 P1 118.4(4) . . ? C15 C14 C13 121.3(5) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 119.5(5) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 120.7(4) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 119.0(4) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C13 C18 O1 123.9(4) . . ? C13 C18 C17 121.9(4) . . ? O1 C18 C17 114.2(4) . . ? N1 C19 C22 110.0(5) . . ? N1 C19 C20 109.0(4) . . ? C22 C19 C20 110.4(5) . . ? N1 C19 C21 107.7(5) . . ? C22 C19 C21 108.6(6) . . ? C20 C19 C21 111.1(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 122.4(5) . . ? C24 C23 P4 114.1(4) . . ? C28 C23 P4 123.4(4) . . ? O2 C24 C23 123.5(4) . . ? O2 C24 C25 120.2(4) . . ? C23 C24 C25 116.3(5) . . ? C26 C25 C24 120.6(5) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 121.7(5) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C28 C27 C26 118.8(5) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C27 C28 C23 120.2(5) . . ? C27 C28 H28 119.9 . . ? C23 C28 H28 119.9 . . ? C30 C29 C34 119.5(5) . . ? C30 C29 P4 118.9(4) . . ? C34 C29 P4 121.3(4) . . ? C29 C30 C31 120.9(5) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C30 C31 C32 118.7(5) . . ? C30 C31 H31 120.7 . . ? C32 C31 H31 120.7 . . ? C33 C32 C31 120.6(5) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 120.7(5) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C29 C34 C33 119.6(5) . . ? C29 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C40 C35 C36 119.6(5) . . ? C40 C35 P4 118.1(4) . . ? C36 C35 P4 121.8(4) . . ? C37 C36 C35 119.5(6) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C38 C37 C36 119.3(6) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C39 C38 C37 121.1(6) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C38 C39 C40 119.8(6) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C35 C40 C39 120.7(6) . . ? C35 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? N2 C41 C44 107.0(5) . . ? N2 C41 C43 108.1(4) . . ? C44 C41 C43 110.5(5) . . ? N2 C41 C42 110.5(4) . . ? C44 C41 C42 112.7(6) . . ? C43 C41 C42 108.0(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47A Pd3 C46A 37.6(5) . . ? C47A Pd3 C46 28.6(5) . . ? C46A Pd3 C46 23.9(9) . . ? C47A Pd3 C47 20.2(7) . . ? C46A Pd3 C47 28.4(5) . . ? C46 Pd3 C47 34.9(4) . . ? C47A Pd3 C45 60.8(5) . . ? C46A Pd3 C45 33.9(5) . . ? C46 Pd3 C45 32.7(4) . . ? C47 Pd3 C45 60.5(5) . . ? C47A Pd3 Cl3 103.1(5) . . ? C46A Pd3 Cl3 133.3(4) . . ? C46 Pd3 Cl3 131.1(4) . . ? C47 Pd3 Cl3 105.3(5) . . ? C45 Pd3 Cl3 163.8(3) . . ? C47A Pd3 Cl3 166.6(5) . 2_667 ? C46A Pd3 Cl3 135.2(5) . 2_667 ? C46 Pd3 Cl3 138.8(4) . 2_667 ? C47 Pd3 Cl3 161.0(6) . 2_667 ? C45 Pd3 Cl3 107.4(3) . 2_667 ? Cl3 Pd3 Cl3 88.29(10) . 2_667 ? Pd3 Cl3 Pd3 91.71(10) . 2_667 ? C46 C45 Pd3 64.4(10) . . ? C46 C45 H45A 120.0 . . ? Pd3 C45 H45A 82.2 . . ? C46 C45 H45B 120.0 . . ? Pd3 C45 H45B 124.6 . . ? H45A C45 H45B 120.0 . . ? C45 C46 C47 124.8(19) . . ? C45 C46 Pd3 82.9(11) . . ? C47 C46 Pd3 72.7(11) . . ? C45 C46 H46 117.6 . . ? C47 C46 H46 117.6 . . ? Pd3 C46 H46 117.0 . . ? C46 C47 Pd3 72.4(11) . . ? C46 C47 H47A 120.0 . . ? Pd3 C47 H47A 81.0 . . ? C46 C47 H47B 120.0 . . ? Pd3 C47 H47B 117.3 . . ? H47A C47 H47B 120.0 . . ? C47A C46A Pd3 70.4(11) . . ? C47A C46A H46A 122.1 . . ? Pd3 C46A H46A 114.1 . . ? C46A C47A Pd3 72.0(11) . . ? C46A C47A H47C 120.0 . . ? Pd3 C47A H47C 85.2 . . ? C46A C47A H47D 120.0 . . ? Pd3 C47A H47D 113.1 . . ? H47C C47A H47D 120.0 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.71 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 4.168 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.154 #===END data_15 _database_code_depnum_ccdc_archive 'CCDC 779805' #TrackingRef '- MSB-94.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Trichloro-1\k^2^,2\k-2-\h^3^-allyl-\m(tert-butyl-[1,3-di- tert-butyl-4-(2-diphenylphosphanylphenoxy)-[1,3,2,4] diazadiphosphetidin-2-yl]amine-1\kP',P":2\kP)dipalladum(II) ; _chemical_name_common ; Trichloro-1kappa$2!,2kappa-2-eta$3!-allyl-mu(tert-butyl-(1,3- di-tert-butyl-4-(2-diphenylphosphanylphenoxy)-(1,3,2,4) diazadiphosphetidin-2-yl)amine-1kappaP',P'':2kappaP)dipalladum(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C33 H47 Cl3 N3 O P3 Pd2' _chemical_formula_sum 'C33 H47 Cl3 N3 O P3 Pd2' _chemical_formula_weight 913.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 10.3506(13) _cell_length_b 14.9616(18) _cell_length_c 24.149(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.218(2) _cell_angle_gamma 90.00 _cell_volume 3738.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8762 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.29 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ?0 _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 1.336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7782 _exptl_absorpt_correction_T_max 0.8725 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 65323 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.33 _reflns_number_total 9288 _reflns_number_gt 8210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS, 2004)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. ; _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) except for that attached to N3 which was placed in the location derived from a difference map. All were included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. Chlorine Cl2, which is attached to the chelated palladium (Pd1), and the tert-butyl groups attached to N1 and N2 are disordered over two sites with approximately equal populations. That attached to N2 shows a simple rotational disorder of the methyl groups while that attached to N1 has two alternate locations for the whole tert-butyl group. One of these latter locations places the group close to Cl2 and suggests that the disorder observed for Cl2 is the result of avoiding this close contact. The allyl group attached to Pd2 is also disordered over two sites 180 deg. apart in an 85:15 ratio. ; _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^)+(0.0496P)^2^+6.7872P] 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 9288 _refine_ls_number_parameters 452 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.124 _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 Pd1 Pd 0.26537(2) 0.482332(17) 0.197948(9) 0.02232(7) Uani 1 1 d D . . Pd2 Pd 0.43533(2) 0.422124(18) 0.422367(10) 0.02550(7) Uani 1 1 d D . . Cl1 Cl 0.06174(7) 0.45644(7) 0.15764(3) 0.0365(2) Uani 1 1 d . A . Cl2 Cl 0.17285(14) 0.51489(12) 0.28379(6) 0.0285(2) Uani 0.5038(16) 1 d PD A 1 Cl2A Cl 0.18750(15) 0.43215(12) 0.28344(6) 0.0285(2) Uani 0.4962(16) 1 d PD A 2 Cl3 Cl 0.61995(8) 0.35255(6) 0.46474(3) 0.03372(19) Uani 1 1 d . B . P1 P 0.34839(7) 0.49430(5) 0.11378(3) 0.01916(15) Uani 1 1 d . A . P2 P 0.45993(7) 0.48264(6) 0.23935(3) 0.02034(15) Uani 1 1 d . A . P3 P 0.53624(7) 0.45958(6) 0.33906(3) 0.02241(16) Uani 1 1 d . A . O1 O 0.57558(19) 0.48273(14) 0.19437(8) 0.0203(4) Uani 1 1 d . . . N1 N 0.5015(2) 0.39764(18) 0.27989(10) 0.0223(5) Uani 1 1 d D . . N2 N 0.5033(2) 0.54616(19) 0.29344(10) 0.0230(5) Uani 1 1 d . . . N3 N 0.6886(2) 0.45820(19) 0.35777(11) 0.0229(5) Uani 1 1 d . . . H3N H 0.6911 0.4434 0.3925 0.027 Uiso 1 1 d R A . C1 C 0.3987(3) 0.3861(2) 0.08825(12) 0.0220(6) Uani 1 1 d . . . C2 C 0.3051(3) 0.3193(2) 0.08285(13) 0.0290(7) Uani 1 1 d . A . H2 H 0.2174 0.3321 0.0905 0.035 Uiso 1 1 calc R . . C3 C 0.3406(4) 0.2349(3) 0.06632(15) 0.0387(9) Uani 1 1 d . . . H3 H 0.2766 0.1897 0.0623 0.046 Uiso 1 1 calc R A . C4 C 0.4675(4) 0.2150(3) 0.05560(15) 0.0415(9) Uani 1 1 d . A . H4 H 0.4909 0.1564 0.0445 0.050 Uiso 1 1 calc R . . C5 C 0.5606(4) 0.2809(3) 0.06108(15) 0.0389(8) Uani 1 1 d . . . H5 H 0.6483 0.2674 0.0538 0.047 Uiso 1 1 calc R A . C6 C 0.5267(3) 0.3667(2) 0.07713(13) 0.0275(7) Uani 1 1 d . A . H6 H 0.5908 0.4119 0.0805 0.033 Uiso 1 1 calc R . . C7 C 0.4925(3) 0.5619(2) 0.11336(12) 0.0216(6) Uani 1 1 d . . . C8 C 0.5127(4) 0.6276(2) 0.07341(14) 0.0301(7) Uani 1 1 d . A . H8 H 0.4459 0.6412 0.0471 0.036 Uiso 1 1 calc R . . C9 C 0.6286(4) 0.6729(2) 0.07173(15) 0.0382(9) Uani 1 1 d . . . H9 H 0.6407 0.7185 0.0450 0.046 Uiso 1 1 calc R A . C10 C 0.7267(4) 0.6519(3) 0.10867(15) 0.0424(10) Uani 1 1 d . A . H10 H 0.8080 0.6808 0.1059 0.051 Uiso 1 1 calc R . . C11 C 0.7078(4) 0.5888(3) 0.15012(14) 0.0353(8) Uani 1 1 d . . . H11 H 0.7751 0.5752 0.1762 0.042 Uiso 1 1 calc R A . C12 C 0.5899(3) 0.5465(2) 0.15265(12) 0.0223(6) Uani 1 1 d . A . C13 C 0.2427(3) 0.5430(2) 0.06141(13) 0.0258(6) Uani 1 1 d . . . C14 C 0.1756(4) 0.6204(3) 0.07440(16) 0.0366(8) Uani 1 1 d . A . H14 H 0.1844 0.6459 0.1103 0.044 Uiso 1 1 calc R . . C15 C 0.0958(4) 0.6601(3) 0.03482(17) 0.0431(10) Uani 1 1 d . . . H15 H 0.0502 0.7131 0.0438 0.052 Uiso 1 1 calc R A . C16 C 0.0817(3) 0.6240(3) -0.01708(16) 0.0419(10) Uani 1 1 d . A . H16 H 0.0266 0.6518 -0.0439 0.050 Uiso 1 1 calc R . . C17 C 0.1478(3) 0.5472(3) -0.03014(15) 0.0382(9) Uani 1 1 d . . . H17 H 0.1382 0.5219 -0.0661 0.046 Uiso 1 1 calc R A . C18 C 0.2288(3) 0.5065(3) 0.00914(14) 0.0303(7) Uani 1 1 d . A . H18 H 0.2744 0.4537 0.0000 0.036 Uiso 1 1 calc R . . C19 C 0.8197(3) 0.4652(2) 0.33448(14) 0.0250(6) Uani 1 1 d . A . C20 C 0.8167(4) 0.4867(3) 0.27461(17) 0.0437(10) Uani 1 1 d . . . H20A H 0.7808 0.4359 0.2538 0.066 Uiso 1 1 calc R A . H20B H 0.9046 0.4988 0.2624 0.066 Uiso 1 1 calc R . . H20C H 0.7625 0.5395 0.2680 0.066 Uiso 1 1 calc R . . C21 C 0.8879(4) 0.5428(3) 0.3671(2) 0.0512(11) Uani 1 1 d . . . H21A H 0.9766 0.5497 0.3543 0.077 Uiso 1 1 calc R A . H21B H 0.8897 0.5289 0.4068 0.077 Uiso 1 1 calc R . . H21C H 0.8403 0.5986 0.3608 0.077 Uiso 1 1 calc R . . C22 C 0.8933(4) 0.3810(3) 0.3486(2) 0.0507(11) Uani 1 1 d . . . H22A H 0.8559 0.3307 0.3277 0.076 Uiso 1 1 calc R A . H22B H 0.8877 0.3691 0.3884 0.076 Uiso 1 1 calc R . . H22C H 0.9840 0.3884 0.3388 0.076 Uiso 1 1 calc R . . C23 C 0.4825(4) 0.6435(3) 0.30331(14) 0.0384(9) Uani 1 1 d D A . C24 C 0.3270(6) 0.6477(5) 0.3111(3) 0.0374(12) Uani 0.521(4) 1 d PD A 1 H24A H 0.2998 0.7102 0.3146 0.056 Uiso 0.521(4) 1 calc PR A 1 H24B H 0.3042 0.6149 0.3447 0.056 Uiso 0.521(4) 1 calc PR A 1 H24C H 0.2832 0.6206 0.2789 0.056 Uiso 0.521(4) 1 calc PR A 1 C25 C 0.5168(7) 0.6899(4) 0.2557(3) 0.0332(11) Uani 0.521(4) 1 d PD A 1 H25A H 0.6095 0.6824 0.2497 0.050 Uiso 0.521(4) 1 calc PR A 1 H25B H 0.4973 0.7535 0.2603 0.050 Uiso 0.521(4) 1 calc PR A 1 H25C H 0.4678 0.6664 0.2238 0.050 Uiso 0.521(4) 1 calc PR A 1 C26 C 0.5378(8) 0.6621(5) 0.3595(3) 0.0427(13) Uani 0.521(4) 1 d PD A 1 H26A H 0.6323 0.6627 0.3580 0.064 Uiso 0.521(4) 1 calc PR A 1 H26B H 0.5102 0.6155 0.3852 0.064 Uiso 0.521(4) 1 calc PR A 1 H26C H 0.5072 0.7204 0.3723 0.064 Uiso 0.521(4) 1 calc PR A 1 C24A C 0.6268(6) 0.6925(5) 0.3100(3) 0.0374(12) Uani 0.479(4) 1 d PD A 2 H24D H 0.6752 0.6839 0.2759 0.056 Uiso 0.479(4) 1 calc PR A 2 H24E H 0.6748 0.6659 0.3413 0.056 Uiso 0.479(4) 1 calc PR A 2 H24F H 0.6153 0.7566 0.3166 0.056 Uiso 0.479(4) 1 calc PR A 2 C25A C 0.4315(8) 0.6947(5) 0.2498(3) 0.0332(11) Uani 0.479(4) 1 d PD A 2 H25D H 0.4308 0.7592 0.2571 0.050 Uiso 0.479(4) 1 calc PR A 2 H25E H 0.3437 0.6746 0.2403 0.050 Uiso 0.479(4) 1 calc PR A 2 H25F H 0.4885 0.6821 0.2189 0.050 Uiso 0.479(4) 1 calc PR A 2 C26A C 0.4115(8) 0.6720(5) 0.3515(3) 0.0427(13) Uani 0.479(4) 1 d PD A 2 H26D H 0.4035 0.7372 0.3514 0.064 Uiso 0.479(4) 1 calc PR A 2 H26E H 0.4579 0.6529 0.3853 0.064 Uiso 0.479(4) 1 calc PR A 2 H26F H 0.3252 0.6450 0.3504 0.064 Uiso 0.479(4) 1 calc PR A 2 C27 C 0.4572(6) 0.3070(5) 0.2777(3) 0.0204(12) Uani 0.518(4) 1 d PD A 1 C28 C 0.4739(8) 0.2776(9) 0.2187(3) 0.0273(18) Uani 0.518(4) 1 d PD A 1 H28A H 0.4092 0.3072 0.1949 0.041 Uiso 0.518(4) 1 calc PR A 1 H28B H 0.4629 0.2127 0.2161 0.041 Uiso 0.518(4) 1 calc PR A 1 H28C H 0.5607 0.2938 0.2067 0.041 Uiso 0.518(4) 1 calc PR A 1 C29 C 0.5476(6) 0.2562(4) 0.3163(3) 0.0297(10) Uani 0.518(4) 1 d PD A 1 H29A H 0.6366 0.2631 0.3039 0.044 Uiso 0.518(4) 1 calc PR A 1 H29B H 0.5243 0.1927 0.3160 0.044 Uiso 0.518(4) 1 calc PR A 1 H29C H 0.5407 0.2798 0.3540 0.044 Uiso 0.518(4) 1 calc PR A 1 C30 C 0.3183(6) 0.2965(4) 0.2956(3) 0.0291(10) Uani 0.518(4) 1 d PD A 1 H30A H 0.3110 0.3151 0.3343 0.044 Uiso 0.518(4) 1 calc PR A 1 H30B H 0.2922 0.2337 0.2918 0.044 Uiso 0.518(4) 1 calc PR A 1 H30C H 0.2618 0.3338 0.2721 0.044 Uiso 0.518(4) 1 calc PR A 1 C27A C 0.5033(7) 0.2934(5) 0.2685(3) 0.0204(12) Uani 0.482(4) 1 d PD A 2 C28A C 0.4268(9) 0.2728(10) 0.2155(4) 0.0273(18) Uani 0.482(4) 1 d PD A 2 H28D H 0.4665 0.3034 0.1843 0.041 Uiso 0.482(4) 1 calc PR A 2 H28E H 0.3376 0.2936 0.2192 0.041 Uiso 0.482(4) 1 calc PR A 2 H28F H 0.4270 0.2082 0.2089 0.041 Uiso 0.482(4) 1 calc PR A 2 C29A C 0.4385(7) 0.2458(4) 0.3169(3) 0.0297(10) Uani 0.482(4) 1 d PD A 2 H29D H 0.3484 0.2654 0.3191 0.044 Uiso 0.482(4) 1 calc PR A 2 H29E H 0.4845 0.2605 0.3516 0.044 Uiso 0.482(4) 1 calc PR A 2 H29F H 0.4411 0.1810 0.3110 0.044 Uiso 0.482(4) 1 calc PR A 2 C30A C 0.6406(6) 0.2579(4) 0.2627(3) 0.0291(10) Uani 0.482(4) 1 d PD A 2 H30D H 0.6374 0.1949 0.2517 0.044 Uiso 0.482(4) 1 calc PR A 2 H30E H 0.6875 0.2635 0.2982 0.044 Uiso 0.482(4) 1 calc PR A 2 H30F H 0.6852 0.2925 0.2344 0.044 Uiso 0.482(4) 1 calc PR A 2 C31 C 0.2511(4) 0.4843(3) 0.41817(16) 0.0421(10) Uani 0.852(8) 1 d PD B 1 H31A H 0.3136 0.5286 0.4275 0.050 Uiso 0.852(8) 1 calc PR B 1 H31B H 0.1956 0.4922 0.3867 0.050 Uiso 0.852(8) 1 calc PR B 1 C32 C 0.2409(4) 0.4085(3) 0.45035(17) 0.0345(10) Uani 0.852(8) 1 d PD B 1 H32 H 0.1784 0.3641 0.4411 0.041 Uiso 0.852(8) 1 calc PR B 1 C33 C 0.3219(3) 0.3975(3) 0.49597(15) 0.0351(8) Uani 0.852(8) 1 d PD B 1 H33A H 0.3842 0.4420 0.5051 0.042 Uiso 0.852(8) 1 calc PR B 1 H33B H 0.3152 0.3455 0.5183 0.042 Uiso 0.852(8) 1 calc PR B 1 C31A C 0.2511(4) 0.4843(3) 0.41817(16) 0.0421(10) Uani 0.148(8) 1 d P B 2 H31C H 0.2792 0.4431 0.3910 0.050 Uiso 0.148(8) 1 calc PR B 2 H31D H 0.2102 0.5384 0.4071 0.050 Uiso 0.148(8) 1 calc PR B 2 C32A C 0.2682(18) 0.4671(14) 0.4692(6) 0.0345(10) Uani 0.148(8) 1 d PD B 2 H32A H 0.2369 0.5123 0.4931 0.041 Uiso 0.148(8) 1 calc PR B 2 C33A C 0.3219(3) 0.3975(3) 0.49597(15) 0.0351(8) Uani 0.148(8) 1 d P B 2 H33C H 0.3560 0.3489 0.4756 0.042 Uiso 0.148(8) 1 calc PR B 2 H33D H 0.3258 0.3968 0.5353 0.042 Uiso 0.148(8) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01287(11) 0.04106(15) 0.01298(11) 0.00078(9) -0.00119(8) -0.00351(9) Pd2 0.01756(12) 0.04307(15) 0.01586(12) 0.00194(9) -0.00005(8) -0.00002(9) Cl1 0.0163(3) 0.0706(6) 0.0224(4) 0.0017(4) -0.0046(3) -0.0054(4) Cl2 0.0190(5) 0.0497(6) 0.0169(5) 0.0005(4) 0.0031(4) -0.0031(4) Cl2A 0.0190(5) 0.0497(6) 0.0169(5) 0.0005(4) 0.0031(4) -0.0031(4) Cl3 0.0243(4) 0.0514(5) 0.0253(4) 0.0097(3) -0.0034(3) 0.0028(3) P1 0.0174(3) 0.0260(4) 0.0141(3) 0.0020(3) -0.0007(3) 0.0018(3) P2 0.0132(3) 0.0332(4) 0.0146(3) 0.0007(3) -0.0016(3) -0.0037(3) P3 0.0127(3) 0.0392(4) 0.0153(4) -0.0006(3) -0.0019(3) -0.0007(3) O1 0.0154(9) 0.0273(11) 0.0181(10) 0.0013(8) 0.0013(8) -0.0026(8) N1 0.0200(12) 0.0325(14) 0.0142(11) 0.0025(10) -0.0044(9) -0.0073(10) N2 0.0185(12) 0.0335(14) 0.0168(12) -0.0031(10) -0.0044(9) 0.0051(10) N3 0.0152(12) 0.0356(14) 0.0177(12) -0.0014(10) -0.0017(9) -0.0010(10) C1 0.0259(15) 0.0269(15) 0.0132(13) -0.0014(11) -0.0028(11) 0.0008(11) C2 0.0315(17) 0.0360(18) 0.0193(15) 0.0019(13) -0.0054(12) -0.0061(13) C3 0.060(3) 0.0326(18) 0.0232(17) 0.0001(14) -0.0074(16) -0.0118(17) C4 0.070(3) 0.0281(18) 0.0263(18) -0.0062(14) -0.0061(17) 0.0085(17) C5 0.044(2) 0.043(2) 0.0294(18) -0.0082(15) -0.0008(15) 0.0145(16) C6 0.0281(16) 0.0334(17) 0.0211(15) -0.0045(12) -0.0013(12) 0.0028(13) C7 0.0244(15) 0.0214(14) 0.0192(14) 0.0003(11) 0.0050(11) -0.0023(11) C8 0.0418(19) 0.0266(16) 0.0221(16) 0.0035(12) 0.0075(13) 0.0000(13) C9 0.063(3) 0.0279(17) 0.0240(17) -0.0004(13) 0.0154(17) -0.0161(16) C10 0.054(2) 0.049(2) 0.0243(17) -0.0078(15) 0.0106(16) -0.0342(19) C11 0.0351(19) 0.051(2) 0.0199(16) -0.0042(14) 0.0012(13) -0.0240(16) C12 0.0265(15) 0.0226(14) 0.0180(14) -0.0019(11) 0.0049(11) -0.0071(11) C13 0.0191(14) 0.0394(17) 0.0191(15) 0.0094(13) 0.0014(11) 0.0050(12) C14 0.0378(19) 0.043(2) 0.0286(18) 0.0073(15) 0.0025(15) 0.0144(16) C15 0.0337(19) 0.052(2) 0.044(2) 0.0221(18) 0.0062(16) 0.0162(17) C16 0.0247(17) 0.064(3) 0.037(2) 0.0278(19) -0.0046(15) 0.0013(16) C17 0.0269(17) 0.063(2) 0.0240(17) 0.0142(16) -0.0069(14) -0.0038(16) C18 0.0232(16) 0.047(2) 0.0206(16) 0.0069(14) -0.0030(12) 0.0008(14) C19 0.0151(13) 0.0294(16) 0.0306(17) 0.0053(13) 0.0010(12) 0.0000(11) C20 0.0233(17) 0.068(3) 0.040(2) 0.0103(19) 0.0007(15) -0.0008(17) C21 0.041(2) 0.052(2) 0.060(3) 0.004(2) -0.015(2) -0.0155(19) C22 0.041(2) 0.052(3) 0.059(3) 0.014(2) 0.007(2) 0.0191(19) C23 0.044(2) 0.042(2) 0.0289(18) -0.0103(15) -0.0116(15) 0.0274(17) C24 0.029(2) 0.028(2) 0.055(3) 0.002(2) 0.003(2) 0.0057(19) C25 0.040(3) 0.019(2) 0.041(3) 0.0024(19) 0.009(3) 0.006(2) C26 0.058(3) 0.028(2) 0.042(3) -0.013(2) -0.012(3) 0.014(2) C24A 0.029(2) 0.028(2) 0.055(3) 0.002(2) 0.003(2) 0.0057(19) C25A 0.040(3) 0.019(2) 0.041(3) 0.0024(19) 0.009(3) 0.006(2) C26A 0.058(3) 0.028(2) 0.042(3) -0.013(2) -0.012(3) 0.014(2) C27 0.016(4) 0.026(3) 0.018(3) 0.0024(19) -0.001(2) -0.009(3) C28 0.037(6) 0.022(2) 0.023(2) -0.0012(16) -0.003(3) -0.005(5) C29 0.038(2) 0.024(2) 0.027(2) 0.0016(17) -0.005(2) -0.0046(19) C30 0.027(2) 0.024(2) 0.037(3) -0.0026(18) 0.0018(19) -0.0031(17) C27A 0.016(4) 0.026(3) 0.018(3) 0.0024(19) -0.001(2) -0.009(3) C28A 0.037(6) 0.022(2) 0.023(2) -0.0012(16) -0.003(3) -0.005(5) C29A 0.038(2) 0.024(2) 0.027(2) 0.0016(17) -0.005(2) -0.0046(19) C30A 0.027(2) 0.024(2) 0.037(3) -0.0026(18) 0.0018(19) -0.0031(17) C31 0.0246(17) 0.071(3) 0.0313(19) 0.0137(18) 0.0067(14) 0.0119(17) C32 0.0213(18) 0.054(3) 0.029(2) -0.0009(18) 0.0058(15) -0.0026(17) C33 0.0311(18) 0.047(2) 0.0277(18) 0.0075(15) 0.0114(14) 0.0014(15) C31A 0.0246(17) 0.071(3) 0.0313(19) 0.0137(18) 0.0067(14) 0.0119(17) C32A 0.0213(18) 0.054(3) 0.029(2) -0.0009(18) 0.0058(15) -0.0026(17) C33A 0.0311(18) 0.047(2) 0.0277(18) 0.0075(15) 0.0114(14) 0.0014(15) _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 Pd1 P2 2.2293(8) . ? Pd1 P1 2.2306(8) . ? Pd1 Cl1 2.3351(8) . ? Pd1 Cl2 2.3528(15) . ? Pd1 Cl2A 2.3551(15) . ? Pd2 C31 2.122(4) . ? Pd2 C32 2.146(4) . ? Pd2 C33 2.182(3) . ? Pd2 C32A 2.192(15) . ? Pd2 P3 2.3541(8) . ? Pd2 Cl3 2.3873(9) . ? P1 C7 1.802(3) . ? P1 C13 1.808(3) . ? P1 C1 1.812(3) . ? P2 O1 1.633(2) . ? P2 N1 1.656(3) . ? P2 N2 1.669(3) . ? P3 N3 1.631(3) . ? P3 N2 1.730(3) . ? P3 N1 1.734(3) . ? O1 C12 1.398(4) . ? N1 C27 1.432(7) . ? N1 C27A 1.584(8) . ? N2 C23 1.492(4) . ? N3 C19 1.484(4) . ? N3 H3N 0.8680 . ? C1 C6 1.389(4) . ? C1 C2 1.396(4) . ? C2 C3 1.377(5) . ? C2 H2 0.9500 . ? C3 C4 1.376(6) . ? C3 H3 0.9500 . ? C4 C5 1.383(6) . ? C4 H4 0.9500 . ? C5 C6 1.388(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.389(4) . ? C7 C8 1.396(4) . ? C8 C9 1.380(5) . ? C8 H8 0.9500 . ? C9 C10 1.373(6) . ? C9 H9 0.9500 . ? C10 C11 1.393(5) . ? C10 H10 0.9500 . ? C11 C12 1.377(4) . ? C11 H11 0.9500 . ? C13 C18 1.380(5) . ? C13 C14 1.390(5) . ? C14 C15 1.384(5) . ? C14 H14 0.9500 . ? C15 C16 1.370(6) . ? C15 H15 0.9500 . ? C16 C17 1.378(6) . ? C16 H16 0.9500 . ? C17 C18 1.392(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.481(5) . ? C19 C22 1.507(5) . ? C19 C21 1.564(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.394(7) . ? C23 C26A 1.453(7) . ? C23 C26 1.487(7) . ? C23 C25A 1.583(7) . ? C23 C24 1.626(7) . ? C23 C24A 1.669(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25A H25D 0.9800 . ? C25A H25E 0.9800 . ? C25A H25F 0.9800 . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 0.9800 . ? C27 C28 1.505(9) . ? C27 C29 1.511(8) . ? C27 C30 1.518(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C27A C28A 1.522(9) . ? C27A C30A 1.527(8) . ? C27A C29A 1.536(8) . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29D 0.9800 . ? C29A H29E 0.9800 . ? C29A H29F 0.9800 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31 C32 1.380(6) . ? C31 H31A 0.9500 . ? C31 H31B 0.9500 . ? C32 C33 1.380(6) . ? C32 H32 0.9500 . ? C33 H33A 0.9500 . ? C33 H33B 0.9500 . ? C32A H32A 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 Pd1 P1 92.68(3) . . ? P2 Pd1 Cl1 170.43(4) . . ? P1 Pd1 Cl1 89.73(3) . . ? P2 Pd1 Cl2 89.15(4) . . ? P1 Pd1 Cl2 163.35(5) . . ? Cl1 Pd1 Cl2 91.20(4) . . ? P2 Pd1 Cl2A 86.00(4) . . ? P1 Pd1 Cl2A 165.93(5) . . ? Cl1 Pd1 Cl2A 89.42(4) . . ? Cl2 Pd1 Cl2A 30.72(6) . . ? C31 Pd2 C32 37.71(16) . . ? C31 Pd2 C33 67.30(14) . . ? C32 Pd2 C33 37.16(15) . . ? C31 Pd2 C32A 34.1(4) . . ? C32 Pd2 C32A 27.3(6) . . ? C33 Pd2 C32A 35.7(4) . . ? C31 Pd2 P3 105.63(10) . . ? C32 Pd2 P3 136.70(12) . . ? C33 Pd2 P3 172.93(10) . . ? C32A Pd2 P3 137.5(4) . . ? C31 Pd2 Cl3 157.20(11) . . ? C32 Pd2 Cl3 124.83(12) . . ? C33 Pd2 Cl3 90.98(10) . . ? C32A Pd2 Cl3 123.1(4) . . ? P3 Pd2 Cl3 96.00(3) . . ? C7 P1 C13 104.97(15) . . ? C7 P1 C1 104.81(14) . . ? C13 P1 C1 107.20(15) . . ? C7 P1 Pd1 112.65(10) . . ? C13 P1 Pd1 115.52(10) . . ? C1 P1 Pd1 110.94(10) . . ? O1 P2 N1 102.07(12) . . ? O1 P2 N2 109.35(12) . . ? N1 P2 N2 84.98(13) . . ? O1 P2 Pd1 111.69(8) . . ? N1 P2 Pd1 118.97(9) . . ? N2 P2 Pd1 125.27(10) . . ? N3 P3 N2 111.25(14) . . ? N3 P3 N1 113.82(13) . . ? N2 P3 N1 80.84(13) . . ? N3 P3 Pd2 101.77(10) . . ? N2 P3 Pd2 129.60(9) . . ? N1 P3 Pd2 119.26(9) . . ? C12 O1 P2 124.79(19) . . ? C27 N1 C27A 21.0(3) . . ? C27 N1 P2 128.8(3) . . ? C27A N1 P2 131.1(3) . . ? C27 N1 P3 126.6(3) . . ? C27A N1 P3 131.8(3) . . ? P2 N1 P3 97.09(14) . . ? C23 N2 P2 130.1(2) . . ? C23 N2 P3 131.0(2) . . ? P2 N2 P3 96.78(15) . . ? C19 N3 P3 141.3(2) . . ? C19 N3 H3N 112.1 . . ? P3 N3 H3N 106.3 . . ? C6 C1 C2 119.7(3) . . ? C6 C1 P1 122.3(2) . . ? C2 C1 P1 117.9(2) . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 120.9(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 120.4(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 119.7(3) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C12 C7 C8 118.1(3) . . ? C12 C7 P1 119.5(2) . . ? C8 C7 P1 122.3(3) . . ? C9 C8 C7 120.6(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.6(3) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 118.7(4) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C11 C12 C7 121.7(3) . . ? C11 C12 O1 117.0(3) . . ? C7 C12 O1 121.2(3) . . ? C18 C13 C14 119.5(3) . . ? C18 C13 P1 122.1(3) . . ? C14 C13 P1 118.4(3) . . ? C15 C14 C13 119.7(4) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 120.9(4) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 119.6(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 120.2(4) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 120.0(4) . . ? C13 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 N3 112.6(3) . . ? C20 C19 C22 113.7(3) . . ? N3 C19 C22 108.5(3) . . ? C20 C19 C21 109.3(3) . . ? N3 C19 C21 105.6(3) . . ? C22 C19 C21 106.6(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C26 124.0(5) . . ? C25 C23 N2 108.3(4) . . ? C26A C23 N2 119.4(4) . . ? C26 C23 N2 105.9(4) . . ? C26A C23 C25A 110.3(4) . . ? N2 C23 C25A 112.9(4) . . ? C25 C23 C24 110.3(4) . . ? C26 C23 C24 104.4(5) . . ? N2 C23 C24 101.7(4) . . ? C26A C23 C24A 105.1(5) . . ? N2 C23 C24A 108.2(3) . . ? C25A C23 C24A 98.5(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? C23 C24A H24D 109.5 . . ? C23 C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C23 C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C23 C25A H25D 109.5 . . ? C23 C25A H25E 109.5 . . ? H25D C25A H25E 109.5 . . ? C23 C25A H25F 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? C23 C26A H26D 109.5 . . ? C23 C26A H26E 109.5 . . ? H26D C26A H26E 109.5 . . ? C23 C26A H26F 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? N1 C27 C28 105.5(6) . . ? N1 C27 C29 105.1(5) . . ? C28 C27 C29 110.8(6) . . ? N1 C27 C30 113.1(5) . . ? C28 C27 C30 111.5(6) . . ? C29 C27 C30 110.6(5) . . ? C28A C27A C30A 108.7(6) . . ? C28A C27A C29A 108.5(6) . . ? C30A C27A C29A 109.4(6) . . ? C28A C27A N1 109.7(7) . . ? C30A C27A N1 111.9(5) . . ? C29A C27A N1 108.6(5) . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29D 109.5 . . ? C27A C29A H29E 109.5 . . ? H29D C29A H29E 109.5 . . ? C27A C29A H29F 109.5 . . ? H29D C29A H29F 109.5 . . ? H29E C29A H29F 109.5 . . ? C27A C30A H30D 109.5 . . ? C27A C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? C27A C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? C32 C31 Pd2 72.1(2) . . ? C32 C31 H31A 120.0 . . ? Pd2 C31 H31A 71.8 . . ? C32 C31 H31B 120.0 . . ? Pd2 C31 H31B 128.3 . . ? H31A C31 H31B 120.0 . . ? C33 C32 C31 119.7(4) . . ? C33 C32 Pd2 72.8(2) . . ? C31 C32 Pd2 70.2(2) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? Pd2 C32 H32 129.1 . . ? C32 C33 Pd2 70.0(2) . . ? C32 C33 H33A 120.0 . . ? Pd2 C33 H33A 72.3 . . ? C32 C33 H33B 120.0 . . ? Pd2 C33 H33B 130.3 . . ? H33A C33 H33B 120.0 . . ? Pd2 C32A H32A 144.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3N Cl3 0.87 2.34 3.123(3) 149.8 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.879 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.117 #===END data_msb344a_1m _database_code_depnum_ccdc_archive 'CCDC 779806' #TrackingRef '- MSB-94.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H48 Au4 Cl6 N2 O2 P4' _chemical_formula_sum 'C45 H48 Au4 Cl6 N2 O2 P4' _chemical_formula_weight 1773.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0756(11) _cell_length_b 18.009(2) _cell_length_c 19.531(3) _cell_angle_alpha 114.773(2) _cell_angle_beta 96.465(2) _cell_angle_gamma 101.395(2) _cell_volume 2772.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 9866 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 29.19 _exptl_crystal_description Slat _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1610 _exptl_absorpt_coefficient_mu 10.894 _exptl_absorpt_correction_type 'integration numerical Gaussian' _exptl_absorpt_correction_T_min 0.0848 _exptl_absorpt_correction_T_max 0.7288 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 20 sec/frame. ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48684 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.00 _reflns_number_total 13235 _reflns_number_gt 10965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _publ_section_references ; Bruker-AXS (2009). APEX2, Version 2009.11-0, Madison, WI. Bruker-AXS (2009a). SAINT, Version 7.68A, Madison, WI Bruker-AXS (2008). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS and SHELXL. Acta Cryst. A64, 112-122. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. Spek, A. L. (2010). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands. ; _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. A small region of density well-removed from the primary molecule and attributable to disordered lattice solvent was removed with the SQUEEZE option of PLATON (Spek, 2010). ; _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^)+(0.0257P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 13235 _refine_ls_number_parameters 547 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.003 _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 Au1 Au 1.039162(18) 0.372581(11) 0.463771(10) 0.03274(5) Uani 1 1 d . . . Au2 Au 0.872658(18) 0.270023(11) 0.280052(10) 0.03244(5) Uani 1 1 d . . . Au3 Au 0.427189(16) -0.033031(10) 0.156821(9) 0.02681(4) Uani 1 1 d . . . Au4 Au 0.498687(18) -0.192527(12) 0.298924(10) 0.03429(5) Uani 1 1 d . . . Cl1 Cl 0.82114(13) 0.41554(8) 0.44787(9) 0.0543(4) Uani 1 1 d . . . Cl2 Cl 0.86926(19) 0.37911(10) 0.25009(10) 0.0723(5) Uani 1 1 d . . . Cl3 Cl 0.17772(11) -0.06834(8) 0.09528(6) 0.0407(3) Uani 1 1 d . . . Cl4 Cl 0.39320(15) -0.13737(10) 0.40332(8) 0.0570(4) Uani 1 1 d . . . P1 P 1.22369(12) 0.31063(7) 0.47542(6) 0.0276(2) Uani 1 1 d . . . P2 P 0.86807(11) 0.14752(7) 0.28005(6) 0.0229(2) Uani 1 1 d . . . P3 P 0.67099(11) 0.00630(7) 0.21682(6) 0.0236(2) Uani 1 1 d . . . P4 P 0.60108(12) -0.25051(7) 0.19675(6) 0.0294(2) Uani 1 1 d . . . O1 O 1.0278(3) 0.14813(17) 0.32791(16) 0.0257(6) Uani 1 1 d . . . O2 O 0.7048(3) -0.07734(18) 0.21625(17) 0.0291(6) Uani 1 1 d . . . N1 N 0.8099(3) 0.0607(2) 0.19117(18) 0.0247(7) Uani 1 1 d . . . N2 N 0.7350(3) 0.0894(2) 0.30450(18) 0.0236(7) Uani 1 1 d . . . C1 C 0.7971(5) 0.0565(3) 0.1110(2) 0.0307(10) Uani 1 1 d . . . C2 C 0.7593(5) -0.0377(3) 0.0535(3) 0.0412(11) Uani 1 1 d . . . H2A H 0.7546 -0.0435 0.0016 0.062 Uiso 1 1 calc R . . H2B H 0.6606 -0.0675 0.0564 0.062 Uiso 1 1 calc R . . H2C H 0.8388 -0.0617 0.0661 0.062 Uiso 1 1 calc R . . C3 C 0.6708(5) 0.0948(3) 0.0935(3) 0.0364(10) Uani 1 1 d . . . H3A H 0.6910 0.1529 0.1331 0.055 Uiso 1 1 calc R . . H3B H 0.5718 0.0617 0.0929 0.055 Uiso 1 1 calc R . . H3C H 0.6692 0.0941 0.0435 0.055 Uiso 1 1 calc R . . C4 C 0.9497(5) 0.1032(3) 0.1045(3) 0.0428(12) Uani 1 1 d . . . H4A H 0.9372 0.1051 0.0553 0.064 Uiso 1 1 calc R . . H4B H 1.0268 0.0737 0.1078 0.064 Uiso 1 1 calc R . . H4C H 0.9825 0.1607 0.1462 0.064 Uiso 1 1 calc R . . C5 C 0.6916(4) 0.1005(3) 0.3797(2) 0.0241(8) Uani 1 1 d . . . C6 C 0.5183(5) 0.0622(3) 0.3635(3) 0.0347(10) Uani 1 1 d . . . H6A H 0.4643 0.0920 0.3424 0.052 Uiso 1 1 calc R . . H6B H 0.4886 0.0678 0.4113 0.052 Uiso 1 1 calc R . . H6C H 0.4918 0.0026 0.3266 0.052 Uiso 1 1 calc R . . C7 C 0.7777(5) 0.0539(3) 0.4125(2) 0.0312(9) Uani 1 1 d . . . H7A H 0.7507 -0.0058 0.3758 0.047 Uiso 1 1 calc R . . H7B H 0.7492 0.0596 0.4606 0.047 Uiso 1 1 calc R . . H7C H 0.8877 0.0781 0.4222 0.047 Uiso 1 1 calc R . . C8 C 0.7337(5) 0.1951(3) 0.4338(2) 0.0311(9) Uani 1 1 d . . . H8A H 0.8422 0.2199 0.4396 0.047 Uiso 1 1 calc R . . H8B H 0.7133 0.2038 0.4839 0.047 Uiso 1 1 calc R . . H8C H 0.6726 0.2221 0.4124 0.047 Uiso 1 1 calc R . . C9 C 1.1738(4) 0.1837(3) 0.3209(2) 0.0242(8) Uani 1 1 d . . . C10 C 1.2196(5) 0.1422(3) 0.2532(2) 0.0317(9) Uani 1 1 d . . . H10 H 1.1539 0.0909 0.2138 0.038 Uiso 1 1 calc R . . C11 C 1.3622(5) 0.1755(3) 0.2424(3) 0.0368(11) Uani 1 1 d . . . H11 H 1.3908 0.1488 0.1951 0.044 Uiso 1 1 calc R . . C12 C 1.4616(5) 0.2487(3) 0.3026(3) 0.0344(10) Uani 1 1 d . . . H12 H 1.5574 0.2726 0.2959 0.041 Uiso 1 1 calc R . . C13 C 1.4196(4) 0.2862(3) 0.3721(3) 0.0318(10) Uani 1 1 d . . . H13 H 1.4902 0.3341 0.4131 0.038 Uiso 1 1 calc R . . C14 C 1.2751(4) 0.2554(2) 0.3839(2) 0.0237(8) Uani 1 1 d . . . C15 C 1.4063(5) 0.3769(3) 0.5414(2) 0.0304(9) Uani 1 1 d . . . C16 C 1.4450(6) 0.4625(3) 0.5690(3) 0.0501(13) Uani 1 1 d . . . H16 H 1.3747 0.4888 0.5556 0.060 Uiso 1 1 calc R . . C17 C 1.5899(7) 0.5120(4) 0.6175(4) 0.0698(19) Uani 1 1 d . . . H17 H 1.6161 0.5714 0.6372 0.084 Uiso 1 1 calc R . . C18 C 1.6936(6) 0.4736(4) 0.6363(3) 0.0591(15) Uani 1 1 d . . . H18 H 1.7911 0.5068 0.6682 0.071 Uiso 1 1 calc R . . C19 C 1.6555(6) 0.3876(4) 0.6088(3) 0.0515(14) Uani 1 1 d . . . H19 H 1.7273 0.3617 0.6214 0.062 Uiso 1 1 calc R . . C20 C 1.5116(5) 0.3384(3) 0.5625(3) 0.0432(12) Uani 1 1 d . . . H20 H 1.4843 0.2793 0.5453 0.052 Uiso 1 1 calc R . . C21 C 1.1657(4) 0.2319(3) 0.5093(2) 0.0302(9) Uani 1 1 d . . . C22 C 1.0757(5) 0.2492(3) 0.5642(3) 0.0365(10) Uani 1 1 d . . . H22 H 1.0411 0.2985 0.5801 0.044 Uiso 1 1 calc R . . C23 C 1.0376(6) 0.1937(4) 0.5953(3) 0.0488(13) Uani 1 1 d . . . H23 H 0.9750 0.2049 0.6316 0.059 Uiso 1 1 calc R . . C24 C 1.0899(5) 0.1221(4) 0.5739(3) 0.0525(15) Uani 1 1 d . . . H24 H 1.0649 0.0854 0.5962 0.063 Uiso 1 1 calc R . . C25 C 1.1791(5) 0.1046(3) 0.5195(3) 0.0461(13) Uani 1 1 d . . . H25 H 1.2148 0.0557 0.5045 0.055 Uiso 1 1 calc R . . C26 C 1.2164(5) 0.1591(3) 0.4869(3) 0.0376(11) Uani 1 1 d . . . H26 H 1.2763 0.1465 0.4493 0.045 Uiso 1 1 calc R . . C27 C 0.8338(4) -0.1061(3) 0.2277(2) 0.0255(9) Uani 1 1 d . . . C28 C 0.9820(5) -0.0555(3) 0.2519(3) 0.0349(10) Uani 1 1 d . . . H28 H 1.0021 0.0022 0.2634 0.042 Uiso 1 1 calc R . . C29 C 1.1012(5) -0.0906(3) 0.2590(3) 0.0389(11) Uani 1 1 d . . . H29 H 1.2034 -0.0564 0.2761 0.047 Uiso 1 1 calc R . . C30 C 1.0720(5) -0.1755(3) 0.2414(3) 0.0372(11) Uani 1 1 d . . . H30 H 1.1540 -0.1993 0.2453 0.045 Uiso 1 1 calc R . . C31 C 0.9219(5) -0.2252(3) 0.2179(3) 0.0353(10) Uani 1 1 d . . . H31 H 0.9023 -0.2831 0.2057 0.042 Uiso 1 1 calc R . . C32 C 0.8003(4) -0.1915(3) 0.2122(2) 0.0256(8) Uani 1 1 d . . . C33 C 0.5003(5) -0.2590(3) 0.1079(3) 0.0368(10) Uani 1 1 d . . . C34 C 0.5706(6) -0.2547(3) 0.0518(3) 0.0517(13) Uani 1 1 d . . . H34 H 0.6775 -0.2476 0.0581 0.062 Uiso 1 1 calc R . . C35 C 0.4865(8) -0.2605(4) -0.0157(4) 0.0706(18) Uani 1 1 d . . . H35 H 0.5368 -0.2570 -0.0542 0.085 Uiso 1 1 calc R . . C36 C 0.3297(9) -0.2713(4) -0.0254(4) 0.071(2) Uani 1 1 d . . . H36 H 0.2722 -0.2757 -0.0707 0.085 Uiso 1 1 calc R . . C37 C 0.2584(8) -0.2756(5) 0.0312(4) 0.083(2) Uani 1 1 d . . . H37 H 0.1513 -0.2830 0.0244 0.100 Uiso 1 1 calc R . . C38 C 0.3400(6) -0.2692(4) 0.0975(3) 0.0572(15) Uani 1 1 d . . . H38 H 0.2893 -0.2715 0.1362 0.069 Uiso 1 1 calc R . . C39 C 0.6138(5) -0.3555(3) 0.1797(3) 0.0347(10) Uani 1 1 d . . . C40 C 0.6213(6) -0.4161(3) 0.1089(3) 0.0491(13) Uani 1 1 d . . . H40 H 0.6117 -0.4050 0.0659 0.059 Uiso 1 1 calc R . . C41 C 0.6431(7) -0.4935(3) 0.1003(3) 0.0583(15) Uani 1 1 d . . . H41 H 0.6489 -0.5344 0.0519 0.070 Uiso 1 1 calc R . . C42 C 0.6563(7) -0.5101(4) 0.1636(4) 0.0633(16) Uani 1 1 d . . . H42 H 0.6707 -0.5625 0.1578 0.076 Uiso 1 1 calc R . . C43 C 0.6484(7) -0.4506(4) 0.2345(4) 0.0598(15) Uani 1 1 d . . . H43 H 0.6579 -0.4618 0.2774 0.072 Uiso 1 1 calc R . . C44 C 0.6264(6) -0.3739(3) 0.2423(3) 0.0469(12) Uani 1 1 d . . . H44 H 0.6198 -0.3333 0.2908 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02808(9) 0.02950(10) 0.04277(10) 0.01722(8) 0.00647(7) 0.01110(7) Au2 0.02956(9) 0.03083(10) 0.04242(10) 0.02350(8) 0.00469(7) 0.00580(7) Au3 0.01953(8) 0.03042(9) 0.02804(9) 0.01277(7) 0.00072(6) 0.00523(6) Au4 0.02682(9) 0.03733(10) 0.03780(10) 0.01658(8) 0.00893(7) 0.00671(7) Cl1 0.0312(6) 0.0387(7) 0.0880(10) 0.0244(7) 0.0029(6) 0.0144(5) Cl2 0.0925(12) 0.0547(10) 0.0887(12) 0.0539(9) 0.0077(9) 0.0182(8) Cl3 0.0233(5) 0.0579(8) 0.0327(6) 0.0157(5) -0.0021(4) 0.0092(5) Cl4 0.0490(7) 0.0792(10) 0.0497(8) 0.0287(7) 0.0251(6) 0.0249(7) P1 0.0246(5) 0.0259(6) 0.0319(6) 0.0131(5) 0.0040(4) 0.0071(5) P2 0.0189(5) 0.0253(6) 0.0260(5) 0.0144(4) 0.0031(4) 0.0035(4) P3 0.0186(5) 0.0258(6) 0.0268(5) 0.0129(4) 0.0019(4) 0.0059(4) P4 0.0273(5) 0.0267(6) 0.0316(6) 0.0125(5) 0.0029(4) 0.0054(5) O1 0.0190(13) 0.0284(16) 0.0309(15) 0.0168(13) 0.0019(11) 0.0032(12) O2 0.0198(14) 0.0249(16) 0.0442(18) 0.0183(14) 0.0027(12) 0.0056(12) N1 0.0179(15) 0.0303(19) 0.0256(18) 0.0151(15) 0.0014(13) 0.0025(14) N2 0.0184(15) 0.0268(18) 0.0275(18) 0.0152(15) 0.0038(13) 0.0041(14) C1 0.028(2) 0.044(3) 0.023(2) 0.018(2) 0.0067(17) 0.009(2) C2 0.041(3) 0.051(3) 0.030(2) 0.016(2) 0.007(2) 0.012(2) C3 0.031(2) 0.050(3) 0.032(2) 0.025(2) 0.0021(18) 0.008(2) C4 0.028(2) 0.066(4) 0.037(3) 0.030(3) 0.0067(19) 0.005(2) C5 0.0189(18) 0.033(2) 0.026(2) 0.0173(18) 0.0041(15) 0.0089(17) C6 0.027(2) 0.046(3) 0.035(2) 0.024(2) 0.0079(18) 0.006(2) C7 0.034(2) 0.033(2) 0.034(2) 0.021(2) 0.0098(18) 0.0119(19) C8 0.034(2) 0.031(2) 0.031(2) 0.0171(19) 0.0063(18) 0.0100(19) C9 0.0172(18) 0.028(2) 0.032(2) 0.0178(18) 0.0039(15) 0.0069(16) C10 0.030(2) 0.033(2) 0.032(2) 0.015(2) 0.0048(18) 0.0108(19) C11 0.036(2) 0.051(3) 0.037(3) 0.026(2) 0.018(2) 0.021(2) C12 0.022(2) 0.043(3) 0.044(3) 0.025(2) 0.0098(18) 0.008(2) C13 0.021(2) 0.030(2) 0.042(3) 0.016(2) 0.0017(17) 0.0041(18) C14 0.0231(19) 0.022(2) 0.028(2) 0.0133(17) 0.0011(15) 0.0063(16) C15 0.029(2) 0.025(2) 0.032(2) 0.0110(18) 0.0020(17) 0.0030(18) C16 0.051(3) 0.034(3) 0.059(3) 0.022(3) -0.007(3) 0.006(2) C17 0.069(4) 0.029(3) 0.081(5) 0.020(3) -0.030(3) -0.013(3) C18 0.046(3) 0.050(4) 0.061(4) 0.023(3) -0.016(3) -0.009(3) C19 0.038(3) 0.052(3) 0.050(3) 0.015(3) -0.008(2) 0.011(2) C20 0.038(3) 0.034(3) 0.048(3) 0.012(2) -0.002(2) 0.009(2) C21 0.024(2) 0.032(2) 0.034(2) 0.017(2) 0.0002(17) 0.0043(18) C22 0.035(2) 0.042(3) 0.032(2) 0.019(2) 0.0033(19) 0.009(2) C23 0.043(3) 0.073(4) 0.036(3) 0.034(3) 0.004(2) 0.008(3) C24 0.037(3) 0.075(4) 0.058(3) 0.052(3) -0.003(2) -0.002(3) C25 0.040(3) 0.050(3) 0.058(3) 0.038(3) -0.004(2) 0.008(2) C26 0.026(2) 0.042(3) 0.053(3) 0.029(2) 0.004(2) 0.009(2) C27 0.0218(19) 0.033(2) 0.026(2) 0.0143(18) 0.0067(15) 0.0125(17) C28 0.024(2) 0.035(3) 0.051(3) 0.024(2) 0.0076(19) 0.0071(19) C29 0.024(2) 0.045(3) 0.053(3) 0.028(2) 0.008(2) 0.008(2) C30 0.028(2) 0.053(3) 0.043(3) 0.028(2) 0.0118(19) 0.021(2) C31 0.038(2) 0.034(3) 0.037(3) 0.016(2) 0.011(2) 0.014(2) C32 0.025(2) 0.027(2) 0.026(2) 0.0130(18) 0.0059(16) 0.0082(17) C33 0.043(3) 0.024(2) 0.033(3) 0.0080(19) -0.006(2) 0.007(2) C34 0.059(3) 0.049(3) 0.038(3) 0.019(3) -0.003(2) 0.004(3) C35 0.101(5) 0.049(4) 0.048(4) 0.022(3) -0.001(3) 0.002(4) C36 0.097(5) 0.039(3) 0.054(4) 0.013(3) -0.031(4) 0.016(3) C37 0.068(4) 0.079(5) 0.083(5) 0.024(4) -0.020(4) 0.031(4) C38 0.046(3) 0.063(4) 0.047(3) 0.011(3) -0.004(2) 0.022(3) C39 0.032(2) 0.027(2) 0.041(3) 0.015(2) 0.0028(19) 0.0040(19) C40 0.060(3) 0.041(3) 0.043(3) 0.015(2) 0.005(2) 0.022(3) C41 0.078(4) 0.038(3) 0.047(3) 0.008(3) 0.002(3) 0.022(3) C42 0.078(4) 0.030(3) 0.080(5) 0.026(3) 0.002(3) 0.016(3) C43 0.084(4) 0.046(4) 0.062(4) 0.038(3) 0.007(3) 0.018(3) C44 0.057(3) 0.040(3) 0.045(3) 0.022(2) 0.008(2) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2286(11) . ? Au1 Cl1 2.2974(12) . ? Au1 Au2 3.2699(6) . ? Au2 P2 2.1983(11) . ? Au2 Cl2 2.2773(14) . ? Au3 P3 2.2072(10) . ? Au3 Cl3 2.2700(10) . ? Au4 P4 2.2341(11) . ? Au4 Cl4 2.2758(12) . ? P1 C15 1.811(4) . ? P1 C14 1.813(4) . ? P1 C21 1.815(4) . ? P2 O1 1.630(3) . ? P2 N2 1.682(3) . ? P2 N1 1.712(3) . ? P3 O2 1.592(3) . ? P3 N2 1.672(3) . ? P3 N1 1.693(3) . ? P4 C33 1.798(5) . ? P4 C39 1.808(5) . ? P4 C32 1.827(4) . ? O1 C9 1.401(4) . ? O2 C27 1.402(4) . ? N1 C1 1.526(5) . ? N2 C5 1.506(5) . ? C1 C4 1.520(6) . ? C1 C3 1.525(6) . ? C1 C2 1.531(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 C8 1.520(6) . ? C5 C6 1.525(5) . ? C5 C7 1.525(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 C10 1.379(5) . ? C9 C14 1.404(5) . ? C10 C11 1.393(6) . ? C10 H10 0.9400 . ? C11 C12 1.387(6) . ? C11 H11 0.9400 . ? C12 C13 1.377(6) . ? C12 H12 0.9400 . ? C13 C14 1.403(5) . ? C13 H13 0.9400 . ? C15 C16 1.355(6) . ? C15 C20 1.407(6) . ? C16 C17 1.404(7) . ? C16 H16 0.9400 . ? C17 C18 1.375(8) . ? C17 H17 0.9400 . ? C18 C19 1.362(7) . ? C18 H18 0.9400 . ? C19 C20 1.383(6) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 C26 1.387(6) . ? C21 C22 1.390(6) . ? C22 C23 1.382(6) . ? C22 H22 0.9400 . ? C23 C24 1.377(7) . ? C23 H23 0.9400 . ? C24 C25 1.377(7) . ? C24 H24 0.9400 . ? C25 C26 1.387(6) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? C27 C28 1.370(5) . ? C27 C32 1.397(6) . ? C28 C29 1.379(6) . ? C28 H28 0.9400 . ? C29 C30 1.380(6) . ? C29 H29 0.9400 . ? C30 C31 1.379(6) . ? C30 H30 0.9400 . ? C31 C32 1.375(6) . ? C31 H31 0.9400 . ? C33 C34 1.352(7) . ? C33 C38 1.410(7) . ? C34 C35 1.397(7) . ? C34 H34 0.9400 . ? C35 C36 1.378(9) . ? C35 H35 0.9400 . ? C36 C37 1.363(10) . ? C36 H36 0.9400 . ? C37 C38 1.366(8) . ? C37 H37 0.9400 . ? C38 H38 0.9400 . ? C39 C40 1.377(6) . ? C39 C44 1.393(6) . ? C40 C41 1.390(7) . ? C40 H40 0.9400 . ? C41 C42 1.385(8) . ? C41 H41 0.9400 . ? C42 C43 1.371(8) . ? C42 H42 0.9400 . ? C43 C44 1.382(7) . ? C43 H43 0.9400 . ? C44 H44 0.9400 . ? 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 P1 Au1 Cl1 170.48(4) . . ? P1 Au1 Au2 104.25(3) . . ? Cl1 Au1 Au2 72.53(4) . . ? P2 Au2 Cl2 166.79(5) . . ? P2 Au2 Au1 91.03(3) . . ? Cl2 Au2 Au1 101.48(5) . . ? P3 Au3 Cl3 177.74(4) . . ? P4 Au4 Cl4 178.19(5) . . ? C15 P1 C14 104.19(18) . . ? C15 P1 C21 103.0(2) . . ? C14 P1 C21 106.19(19) . . ? C15 P1 Au1 118.23(15) . . ? C14 P1 Au1 111.80(13) . . ? C21 P1 Au1 112.36(14) . . ? O1 P2 N2 101.74(15) . . ? O1 P2 N1 110.92(15) . . ? N2 P2 N1 83.89(16) . . ? O1 P2 Au2 113.28(11) . . ? N2 P2 Au2 127.79(12) . . ? N1 P2 Au2 115.44(12) . . ? O2 P3 N2 111.72(16) . . ? O2 P3 N1 113.15(15) . . ? N2 P3 N1 84.81(16) . . ? O2 P3 Au3 105.19(11) . . ? N2 P3 Au3 120.44(11) . . ? N1 P3 Au3 120.89(12) . . ? C33 P4 C39 107.6(2) . . ? C33 P4 C32 106.2(2) . . ? C39 P4 C32 104.01(19) . . ? C33 P4 Au4 115.03(16) . . ? C39 P4 Au4 111.03(15) . . ? C32 P4 Au4 112.19(13) . . ? C9 O1 P2 123.1(2) . . ? C27 O2 P3 137.7(3) . . ? C1 N1 P3 124.1(3) . . ? C1 N1 P2 129.4(3) . . ? P3 N1 P2 94.65(16) . . ? C5 N2 P3 129.3(3) . . ? C5 N2 P2 134.0(3) . . ? P3 N2 P2 96.53(16) . . ? C4 C1 C3 109.4(4) . . ? C4 C1 N1 110.3(3) . . ? C3 C1 N1 111.4(3) . . ? C4 C1 C2 109.1(4) . . ? C3 C1 C2 110.3(4) . . ? N1 C1 C2 106.3(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C8 107.9(3) . . ? N2 C5 C6 108.3(3) . . ? C8 C5 C6 110.1(3) . . ? N2 C5 C7 108.7(3) . . ? C8 C5 C7 111.8(3) . . ? C6 C5 C7 109.9(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 O1 118.1(4) . . ? C10 C9 C14 121.1(4) . . ? O1 C9 C14 120.5(3) . . ? C9 C10 C11 120.6(4) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 119.1(4) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C13 C12 C11 119.8(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 122.3(4) . . ? C12 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C13 C14 C9 116.7(4) . . ? C13 C14 P1 120.1(3) . . ? C9 C14 P1 123.2(3) . . ? C16 C15 C20 119.4(4) . . ? C16 C15 P1 121.3(4) . . ? C20 C15 P1 119.2(3) . . ? C15 C16 C17 120.1(5) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 120.0(5) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C18 C17 120.2(5) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.2(5) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C15 119.9(5) . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? C26 C21 C22 119.3(4) . . ? C26 C21 P1 122.8(3) . . ? C22 C21 P1 117.7(3) . . ? C23 C22 C21 119.6(5) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 121.0(5) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C25 C24 C23 119.6(5) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.1(5) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C21 120.4(5) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? C28 C27 C32 121.8(4) . . ? C28 C27 O2 123.3(4) . . ? C32 C27 O2 114.9(3) . . ? C27 C28 C29 118.8(4) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C28 C29 C30 120.7(4) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 119.6(4) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C32 C31 C30 121.1(4) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C27 117.9(4) . . ? C31 C32 P4 122.1(3) . . ? C27 C32 P4 119.6(3) . . ? C34 C33 C38 118.7(5) . . ? C34 C33 P4 123.5(4) . . ? C38 C33 P4 117.9(4) . . ? C33 C34 C35 120.9(6) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C36 C35 C34 119.7(6) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C37 C36 C35 119.6(6) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 121.0(6) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C37 C38 C33 120.1(6) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? C40 C39 C44 118.7(5) . . ? C40 C39 P4 122.9(4) . . ? C44 C39 P4 118.3(4) . . ? C39 C40 C41 120.6(5) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C42 C41 C40 119.7(5) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C43 C42 C41 120.4(5) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 119.4(5) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C43 C44 C39 121.2(5) . . ? C43 C44 H44 119.4 . . ? C39 C44 H44 119.4 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.967 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.128 # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 491 90 ' ' _platon_squeeze_details ; In a difference map calculated late in the refinement process there appeared a connected set of peaks well-separated from the primary molecule and presumably representing lattice solvent. These could not be readily modeled by any possible solvent molecule, in part because of disorder about the center of symmetry, and so were removed. ; #===END data_17 _database_code_depnum_ccdc_archive 'CCDC 779807' #TrackingRef '- MSB-94.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Trichloro(\m-\h^1^;h^1^;^1^-{tert-butyl-[1,3-di-tert- butyl-4-(2-diphenylphosphanylphenoxy)-[1,3,2,4] diazdiphosphetidine-2-yl]amine}-(\kP;\kP';\kP")) trigold(I) ; _chemical_name_common ; Trichloro(mu-eta$1!;h$1!;$1!-(tert-butyl-(1,3-di-tert-butyl-4- (2-diphenylphosphanylphenoxy)-(1,3,2,4) diazdiphosphetidine-2-yl)amine)- (kappaP;kappaP';kappaP'')) trigold(i) ; _chemical_melting_point ? _chemical_formula_moiety 'C30 H42 Au3 Cl3 N3 O P3' _chemical_formula_sum 'C30 H42 Au3 Cl3 N3 O P3' _chemical_formula_weight 1250.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2971(7) _cell_length_b 12.8937(8) _cell_length_c 16.465(1) _cell_angle_alpha 71.592(1) _cell_angle_beta 71.147(1) _cell_angle_gamma 66.109(1) _cell_volume 2027.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9850 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 28.34 _exptl_crystal_description Needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 11.171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3095 _exptl_absorpt_correction_T_max 0.5305 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36059 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.34 _reflns_number_total 9984 _reflns_number_gt 8714 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SMART (Bruker-AXS, 2000)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. Spek, A. L. (2005). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands. ; _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) execpt for H3n which was placed in the location obtained from a difference map. All were included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached atoms. A region of electron density with the 3 - 4 largest peaks having peak heights approximately 60 - 70% of that of a carbon atom and well-separated from the primary molecule was apparent in the final difference map. Following several unsuccessful attempts to model it as disordered molecules of solvent of crystallization (either dichloromethane or a component of petroleum ether) the region was removed with the SQUEEZE option of PLATON (Spek, 2005). ; _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^)+(0.0585P)^2^+27.5342P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 9984 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Au1 Au 0.55847(4) 0.98647(3) 0.85332(2) 0.03045(10) Uani 1 1 d . . . Au2 Au 1.05998(3) 0.71370(3) 0.842094(19) 0.01954(8) Uani 1 1 d . . . Au3 Au 0.81685(3) 0.74054(2) 0.526130(18) 0.01612(8) Uani 1 1 d . . . Cl1 Cl 0.4455(3) 1.1512(2) 0.9063(2) 0.0517(7) Uani 1 1 d . . . Cl2 Cl 1.2104(2) 0.7281(2) 0.89879(14) 0.0311(5) Uani 1 1 d . . . Cl3 Cl 1.02758(18) 0.73865(18) 0.45405(13) 0.0245(4) Uani 1 1 d . . . P1 P 0.67608(19) 0.83642(17) 0.79142(13) 0.0162(4) Uani 1 1 d . . . P2 P 0.91440(19) 0.70702(17) 0.78237(13) 0.0166(4) Uani 1 1 d . . . P3 P 0.61185(19) 0.73192(17) 0.58258(13) 0.0162(4) Uani 1 1 d . . . O O 0.6043(5) 0.7999(5) 0.7389(4) 0.0202(11) Uani 1 1 d . . . N1 N 0.7597(6) 0.7094(5) 0.8443(4) 0.0161(12) Uani 1 1 d . . . N2 N 0.8258(6) 0.8352(6) 0.7260(4) 0.0168(12) Uani 1 1 d . . . N3 N 0.9725(6) 0.6104(6) 0.7232(4) 0.0214(14) Uani 1 1 d . . . H3N H 0.9165 0.6122 0.7000 0.026 Uiso 1 1 d R . . C1 C 0.7164(8) 0.6198(7) 0.9180(5) 0.0184(14) Uani 1 1 d . . . C2 C 0.7441(10) 0.5125(8) 0.8835(6) 0.0291(19) Uani 1 1 d . . . H2A H 0.8395 0.4803 0.8586 0.044 Uiso 1 1 calc R . . H2B H 0.6948 0.5351 0.8379 0.044 Uiso 1 1 calc R . . H2C H 0.7157 0.4539 0.9319 0.044 Uiso 1 1 calc R . . C3 C 0.7907(9) 0.5880(8) 0.9893(6) 0.0282(18) Uani 1 1 d . . . H3A H 0.8866 0.5628 0.9640 0.042 Uiso 1 1 calc R . . H3B H 0.7684 0.5249 1.0357 0.042 Uiso 1 1 calc R . . H3C H 0.7652 0.6559 1.0140 0.042 Uiso 1 1 calc R . . C4 C 0.5670(9) 0.6717(8) 0.9536(6) 0.0283(18) Uani 1 1 d . . . H4A H 0.5369 0.6152 1.0033 0.042 Uiso 1 1 calc R . . H4B H 0.5203 0.6909 0.9071 0.042 Uiso 1 1 calc R . . H4C H 0.5481 0.7423 0.9731 0.042 Uiso 1 1 calc R . . C5 C 0.8686(8) 0.9366(7) 0.6701(5) 0.0211(15) Uani 1 1 d . . . C6 C 0.8634(10) 1.0128(8) 0.7267(6) 0.0296(19) Uani 1 1 d . . . H6A H 0.7705 1.0554 0.7506 0.044 Uiso 1 1 calc R . . H6B H 0.9092 1.0680 0.6906 0.044 Uiso 1 1 calc R . . H6C H 0.9071 0.9638 0.7750 0.044 Uiso 1 1 calc R . . C7 C 1.0094(8) 0.8908(7) 0.6169(5) 0.0229(16) Uani 1 1 d . . . H7A H 1.0698 0.8461 0.6568 0.034 Uiso 1 1 calc R . . H7B H 1.0369 0.9561 0.5777 0.034 Uiso 1 1 calc R . . H7C H 1.0124 0.8405 0.5818 0.034 Uiso 1 1 calc R . . C8 C 0.7736(8) 1.0047(7) 0.6079(6) 0.0232(16) Uani 1 1 d . . . H8A H 0.7834 0.9558 0.5694 0.035 Uiso 1 1 calc R . . H8B H 0.7948 1.0744 0.5721 0.035 Uiso 1 1 calc R . . H8C H 0.6819 1.0274 0.6424 0.035 Uiso 1 1 calc R . . C9 C 1.1036(8) 0.5157(7) 0.7065(6) 0.0237(16) Uani 1 1 d . . . C10 C 1.1406(9) 0.4387(8) 0.7918(6) 0.0303(19) Uani 1 1 d . . . H10A H 1.1533 0.4841 0.8241 0.045 Uiso 1 1 calc R . . H10B H 1.2232 0.3742 0.7790 0.045 Uiso 1 1 calc R . . H10C H 1.0693 0.4078 0.8276 0.045 Uiso 1 1 calc R . . C11 C 1.2113(8) 0.5680(9) 0.6506(6) 0.0312(19) Uani 1 1 d . . . H11A H 1.1801 0.6261 0.6000 0.047 Uiso 1 1 calc R . . H11B H 1.2920 0.5065 0.6300 0.047 Uiso 1 1 calc R . . H11C H 1.2308 0.6051 0.6860 0.047 Uiso 1 1 calc R . . C12 C 1.0846(9) 0.4455(9) 0.6553(7) 0.033(2) Uani 1 1 d . . . H12A H 1.0150 0.4125 0.6912 0.050 Uiso 1 1 calc R . . H12B H 1.1681 0.3826 0.6409 0.050 Uiso 1 1 calc R . . H12C H 1.0585 0.4963 0.6009 0.050 Uiso 1 1 calc R . . C13 C 0.4857(7) 0.8641(7) 0.7111(6) 0.0200(15) Uani 1 1 d . . . C14 C 0.3749(8) 0.9352(7) 0.7607(6) 0.0236(16) Uani 1 1 d . . . H14 H 0.3783 0.9431 0.8153 0.028 Uiso 1 1 calc R . . C15 C 0.2615(8) 0.9931(7) 0.7294(6) 0.0242(17) Uani 1 1 d . . . H15 H 0.1859 1.0417 0.7627 0.029 Uiso 1 1 calc R . . C16 C 0.2550(8) 0.9822(7) 0.6500(6) 0.0227(16) Uani 1 1 d . . . H16 H 0.1774 1.0260 0.6275 0.027 Uiso 1 1 calc R . . C17 C 0.3629(8) 0.9070(7) 0.6041(6) 0.0218(16) Uani 1 1 d . . . H17 H 0.3568 0.8964 0.5512 0.026 Uiso 1 1 calc R . . C18 C 0.4797(7) 0.8465(7) 0.6332(5) 0.0177(14) Uani 1 1 d . . . C19 C 0.5534(7) 0.7285(7) 0.4930(5) 0.0183(14) Uani 1 1 d . . . C20 C 0.5977(8) 0.7891(7) 0.4088(6) 0.0223(16) Uani 1 1 d . . . H20 H 0.6537 0.8319 0.4004 0.027 Uiso 1 1 calc R . . C21 C 0.5588(8) 0.7860(7) 0.3378(6) 0.0247(17) Uani 1 1 d . . . H21 H 0.5893 0.8261 0.2805 0.030 Uiso 1 1 calc R . . C22 C 0.4762(9) 0.7248(8) 0.3503(6) 0.030(2) Uani 1 1 d . . . H22 H 0.4494 0.7234 0.3017 0.036 Uiso 1 1 calc R . . C23 C 0.4329(9) 0.6661(8) 0.4330(7) 0.0309(19) Uani 1 1 d . . . H23 H 0.3754 0.6248 0.4411 0.037 Uiso 1 1 calc R . . C24 C 0.4716(9) 0.6658(8) 0.5050(6) 0.0272(18) Uani 1 1 d . . . H24 H 0.4426 0.6234 0.5616 0.033 Uiso 1 1 calc R . . C25 C 0.6073(8) 0.5992(7) 0.6633(5) 0.0180(14) Uani 1 1 d . . . C26 C 0.7166(8) 0.4989(7) 0.6559(5) 0.0194(15) Uani 1 1 d . . . H26 H 0.7931 0.5009 0.6099 0.023 Uiso 1 1 calc R . . C27 C 0.7143(9) 0.3949(7) 0.7159(6) 0.0261(17) Uani 1 1 d . . . H27 H 0.7886 0.3259 0.7100 0.031 Uiso 1 1 calc R . . C28 C 0.6030(9) 0.3918(8) 0.7849(6) 0.0269(18) Uani 1 1 d . . . H28 H 0.6020 0.3217 0.8268 0.032 Uiso 1 1 calc R . . C29 C 0.4945(8) 0.4924(8) 0.7909(5) 0.0242(16) Uani 1 1 d . . . H29 H 0.4180 0.4905 0.8367 0.029 Uiso 1 1 calc R . . C30 C 0.4951(8) 0.5952(7) 0.7319(5) 0.0224(16) Uani 1 1 d . . . H30 H 0.4197 0.6635 0.7374 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03409(19) 0.02807(18) 0.03010(19) -0.01164(14) -0.00760(14) -0.00700(14) Au2 0.01839(14) 0.02557(16) 0.01702(15) -0.00141(11) -0.00780(11) -0.00915(12) Au3 0.01438(13) 0.01936(14) 0.01503(14) -0.00352(10) -0.00336(10) -0.00618(10) Cl1 0.0714(19) 0.0358(13) 0.0432(15) -0.0195(12) -0.0089(14) -0.0080(13) Cl2 0.0321(11) 0.0440(12) 0.0273(10) 0.0002(9) -0.0160(9) -0.0213(10) Cl3 0.0166(8) 0.0336(10) 0.0232(9) -0.0072(8) -0.0006(7) -0.0104(8) P1 0.0160(9) 0.0194(9) 0.0149(9) -0.0056(7) -0.0045(7) -0.0054(7) P2 0.0152(8) 0.0193(9) 0.0164(9) -0.0034(7) -0.0066(7) -0.0050(7) P3 0.0145(8) 0.0200(9) 0.0154(9) -0.0034(7) -0.0041(7) -0.0067(7) O 0.017(3) 0.021(3) 0.024(3) -0.008(2) -0.010(2) -0.001(2) N1 0.015(3) 0.017(3) 0.015(3) -0.004(2) -0.003(2) -0.004(2) N2 0.013(3) 0.021(3) 0.015(3) -0.002(2) -0.003(2) -0.006(2) N3 0.015(3) 0.027(3) 0.022(3) -0.012(3) -0.006(3) 0.000(3) C1 0.020(4) 0.024(4) 0.012(3) 0.000(3) -0.007(3) -0.009(3) C2 0.037(5) 0.026(4) 0.022(4) -0.006(3) 0.002(4) -0.016(4) C3 0.027(4) 0.038(5) 0.022(4) 0.001(4) -0.009(3) -0.016(4) C4 0.024(4) 0.037(5) 0.025(4) -0.009(4) 0.000(3) -0.015(4) C5 0.025(4) 0.019(4) 0.022(4) 0.003(3) -0.011(3) -0.012(3) C6 0.043(5) 0.026(4) 0.025(4) -0.004(3) -0.005(4) -0.020(4) C7 0.021(4) 0.027(4) 0.021(4) 0.000(3) -0.009(3) -0.009(3) C8 0.021(4) 0.021(4) 0.022(4) -0.002(3) -0.008(3) -0.002(3) C9 0.015(3) 0.025(4) 0.028(4) -0.007(3) -0.004(3) -0.003(3) C10 0.024(4) 0.030(4) 0.030(5) -0.007(4) -0.010(4) 0.002(3) C11 0.017(4) 0.036(5) 0.032(5) -0.007(4) -0.003(3) -0.003(3) C12 0.023(4) 0.035(5) 0.039(5) -0.021(4) -0.008(4) 0.004(4) C13 0.014(3) 0.019(4) 0.028(4) -0.004(3) -0.009(3) -0.004(3) C14 0.019(4) 0.028(4) 0.026(4) -0.011(3) -0.004(3) -0.007(3) C15 0.014(3) 0.023(4) 0.030(4) -0.008(3) 0.000(3) -0.003(3) C16 0.018(4) 0.020(4) 0.032(4) -0.003(3) -0.014(3) -0.004(3) C17 0.023(4) 0.017(4) 0.027(4) -0.002(3) -0.012(3) -0.005(3) C18 0.012(3) 0.019(3) 0.022(4) -0.001(3) -0.005(3) -0.005(3) C19 0.018(3) 0.022(4) 0.015(3) -0.006(3) -0.006(3) -0.003(3) C20 0.022(4) 0.019(4) 0.024(4) -0.003(3) -0.011(3) -0.002(3) C21 0.027(4) 0.022(4) 0.022(4) -0.008(3) -0.010(3) 0.000(3) C22 0.036(5) 0.024(4) 0.036(5) -0.016(4) -0.021(4) 0.002(4) C23 0.035(5) 0.028(4) 0.042(5) -0.011(4) -0.016(4) -0.014(4) C24 0.029(4) 0.033(5) 0.028(4) -0.004(4) -0.010(4) -0.017(4) C25 0.022(4) 0.019(4) 0.015(3) -0.004(3) -0.004(3) -0.009(3) C26 0.023(4) 0.022(4) 0.014(3) -0.003(3) -0.004(3) -0.009(3) C27 0.029(4) 0.021(4) 0.029(4) -0.008(3) -0.008(4) -0.007(3) C28 0.038(5) 0.027(4) 0.024(4) -0.004(3) -0.010(4) -0.018(4) C29 0.025(4) 0.029(4) 0.019(4) -0.003(3) 0.000(3) -0.015(3) C30 0.021(4) 0.025(4) 0.021(4) -0.003(3) -0.003(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.1988(19) . ? Au1 Cl1 2.270(3) . ? Au2 P2 2.2119(18) . ? Au2 Cl2 2.2768(19) . ? Au3 P3 2.2342(19) . ? Au3 Cl3 2.2851(19) . ? P1 O 1.627(5) . ? P1 N1 1.646(7) . ? P1 N2 1.684(6) . ? P2 N3 1.619(7) . ? P2 N2 1.699(7) . ? P2 N1 1.709(6) . ? P3 C25 1.814(8) . ? P3 C18 1.815(8) . ? P3 C19 1.818(8) . ? O C13 1.397(9) . ? N1 C1 1.495(10) . ? N2 C5 1.501(10) . ? N3 C9 1.498(10) . ? N3 H3N 0.8281 . ? C1 C3 1.517(11) . ? C1 C4 1.528(11) . ? C1 C2 1.538(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.521(12) . ? C5 C6 1.527(11) . ? C5 C8 1.532(11) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.515(12) . ? C9 C11 1.527(12) . ? C9 C12 1.528(12) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.398(11) . ? C13 C14 1.398(11) . ? C14 C15 1.369(12) . ? C14 H14 0.9500 . ? C15 C16 1.386(12) . ? C15 H15 0.9500 . ? C16 C17 1.382(12) . ? C16 H16 0.9500 . ? C17 C18 1.385(11) . ? C17 H17 0.9500 . ? C19 C24 1.390(11) . ? C19 C20 1.402(11) . ? C20 C21 1.392(11) . ? C20 H20 0.9500 . ? C21 C22 1.380(13) . ? C21 H21 0.9500 . ? C22 C23 1.373(14) . ? C22 H22 0.9500 . ? C23 C24 1.388(12) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.386(11) . ? C25 C30 1.405(11) . ? C26 C27 1.397(11) . ? C26 H26 0.9500 . ? C27 C28 1.400(13) . ? C27 H27 0.9500 . ? C28 C29 1.381(13) . ? C28 H28 0.9500 . ? C29 C30 1.375(12) . ? C29 H29 0.9500 . ? C30 H30 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 P1 Au1 Cl1 174.83(10) . . ? P2 Au2 Cl2 177.35(8) . . ? P3 Au3 Cl3 172.37(7) . . ? O P1 N1 102.1(3) . . ? O P1 N2 106.5(3) . . ? N1 P1 N2 84.7(3) . . ? O P1 Au1 117.9(2) . . ? N1 P1 Au1 123.0(2) . . ? N2 P1 Au1 117.1(2) . . ? N3 P2 N2 108.9(3) . . ? N3 P2 N1 109.7(3) . . ? N2 P2 N1 82.3(3) . . ? N3 P2 Au2 115.0(2) . . ? N2 P2 Au2 116.4(2) . . ? N1 P2 Au2 120.0(2) . . ? C25 P3 C18 104.5(4) . . ? C25 P3 C19 105.3(4) . . ? C18 P3 C19 104.8(3) . . ? C25 P3 Au3 113.2(3) . . ? C18 P3 Au3 120.9(2) . . ? C19 P3 Au3 106.9(3) . . ? C13 O P1 128.5(5) . . ? C1 N1 P1 132.3(5) . . ? C1 N1 P2 130.6(5) . . ? P1 N1 P2 97.0(3) . . ? C5 N2 P1 128.4(5) . . ? C5 N2 P2 129.3(5) . . ? P1 N2 P2 95.9(3) . . ? C9 N3 P2 132.8(6) . . ? C9 N3 H3N 114.6 . . ? P2 N3 H3N 112.6 . . ? N1 C1 C3 108.9(6) . . ? N1 C1 C4 108.1(6) . . ? C3 C1 C4 110.3(7) . . ? N1 C1 C2 109.6(6) . . ? C3 C1 C2 111.0(7) . . ? C4 C1 C2 108.9(7) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C7 108.6(6) . . ? N2 C5 C6 111.0(7) . . ? C7 C5 C6 110.0(7) . . ? N2 C5 C8 106.6(6) . . ? C7 C5 C8 109.6(7) . . ? C6 C5 C8 111.0(7) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 111.3(7) . . ? N3 C9 C11 110.0(7) . . ? C10 C9 C11 110.6(7) . . ? N3 C9 C12 105.2(6) . . ? C10 C9 C12 110.0(8) . . ? C11 C9 C12 109.6(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O C13 C18 115.9(7) . . ? O C13 C14 122.8(7) . . ? C18 C13 C14 121.1(7) . . ? C15 C14 C13 118.9(8) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 121.2(8) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 119.1(7) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 121.7(8) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C17 C18 C13 117.8(7) . . ? C17 C18 P3 121.7(6) . . ? C13 C18 P3 119.9(6) . . ? C24 C19 C20 120.0(7) . . ? C24 C19 P3 122.6(6) . . ? C20 C19 P3 117.4(6) . . ? C21 C20 C19 119.5(8) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C22 C21 C20 120.2(8) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 119.9(8) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 121.2(8) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C23 C24 C19 119.1(8) . . ? C23 C24 H24 120.4 . . ? C19 C24 H24 120.4 . . ? C26 C25 C30 119.4(7) . . ? C26 C25 P3 118.8(6) . . ? C30 C25 P3 121.7(6) . . ? C25 C26 C27 120.0(7) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 120.3(8) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C29 C28 C27 118.9(8) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C30 C29 C28 121.4(8) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C25 120.0(8) . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.942 _refine_diff_density_min -5.415 _refine_diff_density_rms 0.275