Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;One electron oxidation of chromium N,N-bis(diarylphosphino)amine and bis(diarylphosphino)methane complexes relevant to ethene trimerisation and tetramerisation. ; _publ_contact_author_name 'Duncan Wass' _publ_contact_author_email DUNCAN.WASS@BRISTOL.AC.UK loop_ _publ_author_name 'Duncan Wass' 'Lucy E. Bowen' 'Mairi F. Haddow' 'A. Orpen' # Attachment 'all.cif' data_lb047sad _database_code_depnum_ccdc_archive 'CCDC 626712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H27 Cr N O4 P2' _chemical_formula_sum 'C31 H27 Cr N O4 P2' _chemical_formula_weight 591.48 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' Cr Cr 0.3209 0.6236 '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 10.795(2) _cell_length_b 15.430(3) _cell_length_c 17.984(4) _cell_angle_alpha 90.51(3) _cell_angle_beta 106.82(3) _cell_angle_gamma 95.17(3) _cell_volume 2853.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5825 _cell_measurement_theta_min 3.307 _cell_measurement_theta_max 27.197 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.877023 _exptl_absorpt_correction_T_max 0.990000 _exptl_absorpt_process_details 'SADABS V2.1' _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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.5 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 32614 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13018 _reflns_number_gt 10688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _computing_publication_material 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^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 13018 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.370 _refine_ls_restrained_S_all 1.370 _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 Cr1 Cr 0.74546(4) 0.77979(2) 0.38335(2) 0.01106(10) Uani 1 1 d . . . Cr2 Cr 0.12415(4) 0.29378(2) 0.11749(2) 0.01037(10) Uani 1 1 d . . . P1 P 0.66853(6) 0.65141(4) 0.30592(4) 0.01142(14) Uani 1 1 d . . . P2 P 0.53841(6) 0.78846(4) 0.29608(4) 0.01006(13) Uani 1 1 d . . . P3 P 0.13553(6) 0.16773(4) 0.19080(4) 0.01034(13) Uani 1 1 d . . . P4 P 0.00631(6) 0.29842(4) 0.20739(3) 0.00986(13) Uani 1 1 d . . . N1 N 0.51589(19) 0.68194(13) 0.26354(11) 0.0118(4) Uani 1 1 d . . . N2 N 0.04765(19) 0.20179(12) 0.24929(11) 0.0105(4) Uani 1 1 d . . . O1 O 0.61896(17) 0.71029(12) 0.50354(10) 0.0196(4) Uani 1 1 d . . . O2 O 0.92432(19) 0.87927(13) 0.30442(11) 0.0298(5) Uani 1 1 d . . . O3 O 0.7591(2) 0.95742(13) 0.45812(12) 0.0303(5) Uani 1 1 d . . . O4 O 0.99524(19) 0.72359(15) 0.48843(12) 0.0346(5) Uani 1 1 d . . . O5 O -0.09101(17) 0.24747(12) -0.03214(10) 0.0205(4) Uani 1 1 d . . . O6 O 0.36097(17) 0.38408(12) 0.23622(11) 0.0238(4) Uani 1 1 d . . . O7 O 0.09956(19) 0.47905(12) 0.06913(11) 0.0252(5) Uani 1 1 d . . . O8 O 0.29132(18) 0.23859(14) 0.02051(11) 0.0293(5) Uani 1 1 d . . . C1 C 0.6633(2) 0.73479(16) 0.45560(14) 0.0140(5) Uani 1 1 d . . . C2 C 0.8513(3) 0.83841(17) 0.32858(15) 0.0183(6) Uani 1 1 d . . . C3 C 0.7546(3) 0.88893(17) 0.43074(15) 0.0175(6) Uani 1 1 d . . . C4 C 0.8992(3) 0.74486(18) 0.44792(15) 0.0195(6) Uani 1 1 d . . . C5 C 0.4151(2) 0.63377(16) 0.19677(14) 0.0163(5) Uani 1 1 d . . . H5 H 0.4306 0.5709 0.2015 0.020 Uiso 1 1 calc R . . C6 C 0.4260(3) 0.65995(18) 0.11668(14) 0.0214(6) Uani 1 1 d . . . H6A H 0.3922 0.7166 0.1044 0.032 Uiso 1 1 calc R . . H6B H 0.3753 0.6161 0.0772 0.032 Uiso 1 1 calc R . . H6C H 0.5174 0.6639 0.1172 0.032 Uiso 1 1 calc R . . C7 C 0.2781(3) 0.63996(18) 0.20146(16) 0.0227(6) Uani 1 1 d . . . H7A H 0.2686 0.6129 0.2488 0.034 Uiso 1 1 calc R . . H7B H 0.2156 0.6097 0.1559 0.034 Uiso 1 1 calc R . . H7C H 0.2617 0.7013 0.2026 0.034 Uiso 1 1 calc R . . C8 C 0.6458(2) 0.54968(16) 0.35308(13) 0.0132(5) Uani 1 1 d . . . C9 C 0.7479(3) 0.49673(16) 0.37361(14) 0.0169(5) Uani 1 1 d . . . H9 H 0.8257 0.5122 0.3602 0.020 Uiso 1 1 calc R . . C10 C 0.7356(3) 0.42119(17) 0.41375(14) 0.0196(6) Uani 1 1 d . . . H10 H 0.8050 0.3851 0.4276 0.024 Uiso 1 1 calc R . . C11 C 0.6223(3) 0.39848(17) 0.43360(14) 0.0202(6) Uani 1 1 d . . . H11 H 0.6143 0.3469 0.4610 0.024 Uiso 1 1 calc R . . C12 C 0.5209(3) 0.45067(17) 0.41359(15) 0.0205(6) Uani 1 1 d . . . H12 H 0.4432 0.4349 0.4271 0.025 Uiso 1 1 calc R . . C13 C 0.5328(3) 0.52641(17) 0.37351(14) 0.0165(5) Uani 1 1 d . . . H13 H 0.4633 0.5624 0.3601 0.020 Uiso 1 1 calc R . . C14 C 0.7268(3) 0.61396(17) 0.22615(14) 0.0172(6) Uani 1 1 d . . . C15 C 0.8163(3) 0.66686(18) 0.20027(16) 0.0234(6) Uani 1 1 d . . . H15 H 0.8518 0.7212 0.2264 0.028 Uiso 1 1 calc R . . C16 C 0.8541(3) 0.6407(2) 0.13645(17) 0.0323(8) Uani 1 1 d . . . H16 H 0.9161 0.6767 0.1196 0.039 Uiso 1 1 calc R . . C17 C 0.8013(3) 0.5622(2) 0.09764(17) 0.0369(8) Uani 1 1 d . . . H17 H 0.8257 0.5450 0.0534 0.044 Uiso 1 1 calc R . . C18 C 0.7127(3) 0.5083(2) 0.12290(16) 0.0294(7) Uani 1 1 d . . . H18 H 0.6771 0.4542 0.0963 0.035 Uiso 1 1 calc R . . C19 C 0.6764(3) 0.53370(17) 0.18727(15) 0.0206(6) Uani 1 1 d . . . H19 H 0.6168 0.4963 0.2050 0.025 Uiso 1 1 calc R . . C20 C 0.4159(2) 0.81414(15) 0.34277(13) 0.0114(5) Uani 1 1 d . . . C21 C 0.3398(2) 0.75269(17) 0.37053(14) 0.0168(5) Uani 1 1 d . . . H21 H 0.3435 0.6925 0.3608 0.020 Uiso 1 1 calc R . . C22 C 0.2586(3) 0.77809(18) 0.41218(15) 0.0206(6) Uani 1 1 d . . . H22 H 0.2056 0.7353 0.4297 0.025 Uiso 1 1 calc R . . C23 C 0.2543(3) 0.86567(18) 0.42854(15) 0.0204(6) Uani 1 1 d . . . H23 H 0.1980 0.8830 0.4567 0.024 Uiso 1 1 calc R . . C24 C 0.3327(3) 0.92735(18) 0.40346(15) 0.0206(6) Uani 1 1 d . . . H24 H 0.3320 0.9873 0.4157 0.025 Uiso 1 1 calc R . . C25 C 0.4125(2) 0.90221(16) 0.36048(14) 0.0152(5) Uani 1 1 d . . . H25 H 0.4652 0.9452 0.3430 0.018 Uiso 1 1 calc R . . C26 C 0.4978(2) 0.85080(15) 0.20778(14) 0.0114(5) Uani 1 1 d . . . C27 C 0.3720(2) 0.87300(16) 0.17311(14) 0.0142(5) Uani 1 1 d . . . H27 H 0.3084 0.8641 0.2000 0.017 Uiso 1 1 calc R . . C28 C 0.3386(2) 0.90787(16) 0.10009(14) 0.0156(5) Uani 1 1 d . . . H28 H 0.2524 0.9225 0.0773 0.019 Uiso 1 1 calc R . . C29 C 0.4305(3) 0.92145(17) 0.06037(15) 0.0207(6) Uani 1 1 d . . . H29 H 0.4072 0.9441 0.0098 0.025 Uiso 1 1 calc R . . C30 C 0.5569(3) 0.90171(19) 0.09485(16) 0.0234(6) Uani 1 1 d . . . H30 H 0.6206 0.9120 0.0681 0.028 Uiso 1 1 calc R . . C31 C 0.5906(3) 0.86705(17) 0.16802(15) 0.0181(6) Uani 1 1 d . . . H31 H 0.6775 0.8542 0.1913 0.022 Uiso 1 1 calc R . . C32 C -0.0144(2) 0.26079(16) 0.02772(14) 0.0135(5) Uani 1 1 d . . . C33 C 0.2716(2) 0.34624(16) 0.19346(14) 0.0145(5) Uani 1 1 d . . . C34 C 0.1069(2) 0.40739(17) 0.08548(14) 0.0160(5) Uani 1 1 d . . . C35 C 0.2292(2) 0.26096(18) 0.05820(14) 0.0176(6) Uani 1 1 d . . . C36 C -0.0183(2) 0.15459(17) 0.30200(14) 0.0158(5) Uani 1 1 d . . . H36 H -0.0519 0.2002 0.3288 0.019 Uiso 1 1 calc R . . C37 C 0.0749(3) 0.10855(18) 0.36572(15) 0.0224(6) Uani 1 1 d . . . H37A H 0.1138 0.0647 0.3423 0.034 Uiso 1 1 calc R . . H37B H 0.0274 0.0801 0.3992 0.034 Uiso 1 1 calc R . . H37C H 0.1436 0.1512 0.3968 0.034 Uiso 1 1 calc R . . C38 C -0.1369(2) 0.09286(17) 0.25866(15) 0.0193(6) Uani 1 1 d . . . H38A H -0.1933 0.1236 0.2165 0.029 Uiso 1 1 calc R . . H38B H -0.1852 0.0729 0.2948 0.029 Uiso 1 1 calc R . . H38C H -0.1080 0.0426 0.2369 0.029 Uiso 1 1 calc R . . C39 C 0.0643(2) 0.05756(16) 0.15441(14) 0.0121(5) Uani 1 1 d . . . C40 C 0.1054(2) -0.01580(16) 0.19482(14) 0.0138(5) Uani 1 1 d . . . H40 H 0.1787 -0.0101 0.2397 0.017 Uiso 1 1 calc R . . C41 C 0.0402(2) -0.09746(16) 0.17019(15) 0.0165(5) Uani 1 1 d . . . H41 H 0.0686 -0.1475 0.1982 0.020 Uiso 1 1 calc R . . C42 C -0.0669(3) -0.10557(17) 0.10427(15) 0.0191(6) Uani 1 1 d . . . H42 H -0.1127 -0.1612 0.0878 0.023 Uiso 1 1 calc R . . C43 C -0.1068(3) -0.03334(17) 0.06282(15) 0.0191(6) Uani 1 1 d . . . H43 H -0.1790 -0.0393 0.0173 0.023 Uiso 1 1 calc R . . C44 C -0.0410(2) 0.04832(17) 0.08775(14) 0.0158(5) Uani 1 1 d . . . H44 H -0.0683 0.0980 0.0590 0.019 Uiso 1 1 calc R . . C45 C 0.2982(2) 0.14821(15) 0.25048(14) 0.0123(5) Uani 1 1 d . . . C46 C 0.3524(2) 0.18197(17) 0.32591(15) 0.0176(6) Uani 1 1 d . . . H46 H 0.3026 0.2146 0.3496 0.021 Uiso 1 1 calc R . . C47 C 0.4793(2) 0.16827(17) 0.36699(16) 0.0200(6) Uani 1 1 d . . . H47 H 0.5146 0.1900 0.4192 0.024 Uiso 1 1 calc R . . C48 C 0.5540(2) 0.12334(17) 0.33232(16) 0.0201(6) Uani 1 1 d . . . H48 H 0.6403 0.1136 0.3607 0.024 Uiso 1 1 calc R . . C49 C 0.5026(2) 0.09235(16) 0.25584(16) 0.0188(6) Uani 1 1 d . . . H49 H 0.5548 0.0631 0.2312 0.023 Uiso 1 1 calc R . . C50 C 0.3754(2) 0.10407(16) 0.21550(15) 0.0156(5) Uani 1 1 d . . . H50 H 0.3403 0.0819 0.1635 0.019 Uiso 1 1 calc R . . C51 C -0.1699(2) 0.29505(15) 0.18609(14) 0.0115(5) Uani 1 1 d . . . C52 C -0.2512(2) 0.26523(16) 0.11345(14) 0.0159(5) Uani 1 1 d . . . H52 H -0.2144 0.2501 0.0737 0.019 Uiso 1 1 calc R . . C53 C -0.3851(2) 0.25746(17) 0.09864(15) 0.0193(6) Uani 1 1 d . . . H53 H -0.4397 0.2374 0.0488 0.023 Uiso 1 1 calc R . . C54 C -0.4394(2) 0.27922(18) 0.15709(15) 0.0195(6) Uani 1 1 d . . . H54 H -0.5311 0.2734 0.1473 0.023 Uiso 1 1 calc R . . C55 C -0.3590(2) 0.30939(16) 0.22961(15) 0.0163(5) Uani 1 1 d . . . H55 H -0.3959 0.3243 0.2694 0.020 Uiso 1 1 calc R . . C56 C -0.2259(2) 0.31764(15) 0.24380(14) 0.0125(5) Uani 1 1 d . . . H56 H -0.1715 0.3389 0.2933 0.015 Uiso 1 1 calc R . . C57 C 0.0590(2) 0.38395(15) 0.28336(13) 0.0106(5) Uani 1 1 d . . . C58 C 0.0329(2) 0.46821(16) 0.26062(14) 0.0154(5) Uani 1 1 d . . . H58 H -0.0105 0.4782 0.2078 0.018 Uiso 1 1 calc R . . C59 C 0.0699(2) 0.53751(17) 0.31466(15) 0.0176(6) Uani 1 1 d . . . H59 H 0.0519 0.5948 0.2989 0.021 Uiso 1 1 calc R . . C60 C 0.1332(3) 0.52283(17) 0.39148(15) 0.0205(6) Uani 1 1 d . . . H60 H 0.1574 0.5701 0.4287 0.025 Uiso 1 1 calc R . . C61 C 0.1613(3) 0.43977(18) 0.41441(15) 0.0228(6) Uani 1 1 d . . . H61 H 0.2060 0.4302 0.4671 0.027 Uiso 1 1 calc R . . C62 C 0.1241(2) 0.37015(17) 0.36038(14) 0.0166(5) Uani 1 1 d . . . H62 H 0.1434 0.3131 0.3762 0.020 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 Cr1 0.0110(2) 0.0101(2) 0.0127(2) 0.00166(16) 0.00448(16) 0.00067(15) Cr2 0.0085(2) 0.0116(2) 0.01029(19) -0.00206(15) 0.00214(15) -0.00064(15) P1 0.0146(3) 0.0094(3) 0.0123(3) 0.0017(2) 0.0066(3) 0.0029(2) P2 0.0113(3) 0.0080(3) 0.0117(3) 0.0004(2) 0.0046(2) 0.0013(2) P3 0.0086(3) 0.0101(3) 0.0115(3) -0.0023(2) 0.0017(2) 0.0007(2) P4 0.0084(3) 0.0100(3) 0.0105(3) -0.0022(2) 0.0020(2) 0.0004(2) N1 0.0141(11) 0.0081(10) 0.0136(10) -0.0006(8) 0.0046(8) 0.0019(8) N2 0.0115(10) 0.0084(10) 0.0126(10) -0.0002(8) 0.0045(8) 0.0025(8) O1 0.0222(10) 0.0205(10) 0.0179(9) 0.0024(8) 0.0091(8) 0.0006(8) O2 0.0296(12) 0.0303(12) 0.0322(11) 0.0078(10) 0.0160(10) -0.0062(9) O3 0.0400(13) 0.0169(11) 0.0311(11) -0.0071(9) 0.0059(10) 0.0028(9) O4 0.0173(11) 0.0489(14) 0.0370(12) 0.0211(11) 0.0043(9) 0.0099(10) O5 0.0165(10) 0.0266(11) 0.0150(9) -0.0039(8) 0.0004(8) -0.0010(8) O6 0.0158(10) 0.0275(11) 0.0237(10) -0.0101(9) 0.0005(8) -0.0027(8) O7 0.0372(12) 0.0161(10) 0.0208(10) 0.0022(8) 0.0061(9) 0.0015(9) O8 0.0142(10) 0.0524(14) 0.0206(10) -0.0161(10) 0.0051(8) 0.0013(9) C1 0.0133(13) 0.0122(13) 0.0151(12) -0.0018(10) 0.0019(10) 0.0013(10) C2 0.0199(14) 0.0173(14) 0.0178(13) 0.0022(11) 0.0055(11) 0.0012(11) C3 0.0186(14) 0.0172(14) 0.0153(13) 0.0013(11) 0.0037(11) -0.0013(11) C4 0.0170(14) 0.0225(15) 0.0206(14) 0.0046(11) 0.0094(11) -0.0031(11) C5 0.0192(14) 0.0109(12) 0.0164(13) -0.0029(10) 0.0022(11) -0.0008(10) C6 0.0299(16) 0.0181(14) 0.0142(13) -0.0035(11) 0.0032(12) 0.0023(12) C7 0.0180(14) 0.0224(15) 0.0244(14) -0.0058(12) 0.0035(11) -0.0055(11) C8 0.0217(14) 0.0106(12) 0.0078(11) 0.0001(9) 0.0052(10) 0.0006(10) C9 0.0232(14) 0.0150(13) 0.0141(12) -0.0022(10) 0.0074(11) 0.0033(11) C10 0.0335(16) 0.0133(13) 0.0114(12) -0.0026(10) 0.0039(11) 0.0080(12) C11 0.0353(17) 0.0090(12) 0.0117(12) -0.0008(10) 0.0016(12) -0.0042(11) C12 0.0257(15) 0.0168(14) 0.0173(13) -0.0012(11) 0.0069(11) -0.0086(11) C13 0.0199(14) 0.0155(13) 0.0134(12) 0.0003(10) 0.0040(10) 0.0005(11) C14 0.0246(15) 0.0165(13) 0.0144(12) 0.0051(10) 0.0089(11) 0.0116(11) C15 0.0342(17) 0.0166(14) 0.0277(15) 0.0096(12) 0.0188(13) 0.0129(12) C16 0.048(2) 0.0283(17) 0.0365(17) 0.0180(14) 0.0325(16) 0.0210(15) C17 0.068(2) 0.0356(19) 0.0223(16) 0.0138(14) 0.0285(16) 0.0352(17) C18 0.049(2) 0.0266(16) 0.0175(14) 0.0021(12) 0.0121(14) 0.0239(15) C19 0.0310(16) 0.0175(14) 0.0163(13) 0.0037(11) 0.0086(12) 0.0117(12) C20 0.0106(12) 0.0124(12) 0.0120(12) -0.0005(10) 0.0041(10) 0.0027(10) C21 0.0189(14) 0.0125(13) 0.0208(13) 0.0000(11) 0.0079(11) 0.0034(10) C22 0.0191(14) 0.0204(14) 0.0252(15) 0.0033(12) 0.0114(12) 0.0011(11) C23 0.0171(14) 0.0280(16) 0.0198(14) -0.0020(12) 0.0095(11) 0.0083(12) C24 0.0249(15) 0.0173(14) 0.0220(14) -0.0018(11) 0.0084(12) 0.0091(11) C25 0.0181(13) 0.0119(13) 0.0162(12) -0.0004(10) 0.0060(10) 0.0013(10) C26 0.0141(12) 0.0061(11) 0.0140(12) -0.0008(9) 0.0045(10) 0.0004(9) C27 0.0130(13) 0.0116(12) 0.0180(13) -0.0009(10) 0.0054(10) -0.0011(10) C28 0.0158(13) 0.0115(12) 0.0176(13) 0.0006(10) 0.0013(10) 0.0038(10) C29 0.0250(15) 0.0182(14) 0.0183(13) 0.0071(11) 0.0049(11) 0.0037(11) C30 0.0216(15) 0.0294(16) 0.0231(14) 0.0086(12) 0.0117(12) 0.0044(12) C31 0.0130(13) 0.0198(14) 0.0225(14) 0.0044(11) 0.0063(11) 0.0025(11) C32 0.0117(12) 0.0130(13) 0.0176(13) 0.0002(10) 0.0073(10) 0.0014(10) C33 0.0142(13) 0.0153(13) 0.0155(12) -0.0002(10) 0.0062(10) 0.0028(10) C34 0.0144(13) 0.0213(15) 0.0107(12) -0.0033(11) 0.0019(10) -0.0009(11) C35 0.0116(13) 0.0242(15) 0.0116(12) -0.0056(11) -0.0035(10) -0.0027(11) C36 0.0190(14) 0.0173(13) 0.0134(12) 0.0022(10) 0.0081(11) 0.0027(11) C37 0.0263(16) 0.0219(15) 0.0191(14) 0.0041(12) 0.0063(12) 0.0033(12) C38 0.0183(14) 0.0139(13) 0.0267(14) 0.0032(11) 0.0090(12) -0.0006(11) C39 0.0100(12) 0.0128(12) 0.0138(12) -0.0046(10) 0.0048(10) -0.0008(10) C40 0.0099(12) 0.0138(13) 0.0170(13) -0.0014(10) 0.0033(10) 0.0002(10) C41 0.0161(13) 0.0122(13) 0.0237(14) 0.0018(11) 0.0094(11) 0.0021(10) C42 0.0215(14) 0.0130(13) 0.0237(14) -0.0075(11) 0.0104(12) -0.0059(11) C43 0.0182(14) 0.0194(14) 0.0168(13) -0.0037(11) 0.0021(11) -0.0034(11) C44 0.0166(13) 0.0146(13) 0.0152(13) -0.0002(10) 0.0035(10) -0.0010(10) C45 0.0103(12) 0.0079(12) 0.0171(12) 0.0004(10) 0.0018(10) -0.0006(9) C46 0.0129(13) 0.0168(14) 0.0212(13) -0.0024(11) 0.0018(11) 0.0030(10) C47 0.0135(13) 0.0192(14) 0.0208(14) -0.0031(11) -0.0043(11) -0.0019(11) C48 0.0087(13) 0.0142(13) 0.0335(16) 0.0019(12) 0.0001(11) 0.0002(10) C49 0.0130(13) 0.0124(13) 0.0330(15) -0.0008(11) 0.0097(12) 0.0016(10) C50 0.0154(13) 0.0103(12) 0.0203(13) -0.0009(10) 0.0039(11) 0.0009(10) C51 0.0106(12) 0.0059(11) 0.0173(12) 0.0000(10) 0.0030(10) 0.0003(9) C52 0.0146(13) 0.0184(14) 0.0157(13) -0.0026(11) 0.0052(10) 0.0051(10) C53 0.0121(13) 0.0248(15) 0.0173(13) -0.0067(11) -0.0003(10) -0.0003(11) C54 0.0076(12) 0.0263(15) 0.0237(14) -0.0050(12) 0.0036(11) 0.0007(11) C55 0.0132(13) 0.0176(13) 0.0192(13) -0.0030(11) 0.0066(10) 0.0014(10) C56 0.0140(13) 0.0094(12) 0.0131(12) -0.0017(10) 0.0026(10) -0.0004(10) C57 0.0074(11) 0.0114(12) 0.0140(12) -0.0028(10) 0.0053(9) -0.0013(9) C58 0.0167(13) 0.0153(13) 0.0131(12) -0.0005(10) 0.0034(10) -0.0008(10) C59 0.0194(14) 0.0109(13) 0.0215(14) -0.0018(11) 0.0059(11) -0.0029(10) C60 0.0210(14) 0.0166(14) 0.0218(14) -0.0090(11) 0.0046(11) -0.0035(11) C61 0.0255(15) 0.0233(15) 0.0147(13) -0.0055(11) -0.0023(11) 0.0044(12) C62 0.0172(14) 0.0136(13) 0.0175(13) -0.0023(11) 0.0021(11) 0.0038(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 Cr1 C4 1.858(3) . yes Cr1 C3 1.862(3) . yes Cr1 C1 1.878(3) . yes Cr1 C2 1.891(3) . yes Cr1 P2 2.3461(11) . yes Cr1 P1 2.3533(11) . yes Cr2 C34 1.858(3) . yes Cr2 C35 1.863(3) . yes Cr2 C33 1.883(3) . yes Cr2 C32 1.885(3) . yes Cr2 P4 2.3326(9) . yes Cr2 P3 2.3518(10) . yes P1 N1 1.714(2) . yes P1 C8 1.822(3) . yes P1 C14 1.833(3) . yes P2 N1 1.712(2) . yes P2 C26 1.827(3) . yes P2 C20 1.828(3) . yes P3 N2 1.715(2) . yes P3 C45 1.827(3) . yes P3 C39 1.834(2) . yes P4 N2 1.713(2) . yes P4 C57 1.821(2) . yes P4 C51 1.824(2) . yes N1 C5 1.504(3) . yes N2 C36 1.499(3) . yes O1 C1 1.152(3) . ? O2 C2 1.149(3) . ? O3 C3 1.153(3) . ? O4 C4 1.158(3) . ? O5 C32 1.156(3) . ? O6 C33 1.151(3) . ? O7 C34 1.150(3) . ? O8 C35 1.153(3) . ? C5 C7 1.516(4) . ? C5 C6 1.534(3) . ? C5 H5 1.0000 . ? 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 C13 1.391(3) . ? C8 C9 1.397(4) . ? C9 C10 1.393(4) . ? C9 H9 0.9500 . ? C10 C11 1.387(4) . ? C10 H10 0.9500 . ? C11 C12 1.383(4) . ? C11 H11 0.9500 . ? C12 C13 1.394(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.393(4) . ? C14 C19 1.401(4) . ? C15 C16 1.393(4) . ? C15 H15 0.9500 . ? C16 C17 1.382(5) . ? C16 H16 0.9500 . ? C17 C18 1.387(5) . ? C17 H17 0.9500 . ? C18 C19 1.389(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.389(3) . ? C20 C25 1.399(3) . ? C21 C22 1.385(4) . ? C21 H21 0.9500 . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 C24 1.381(4) . ? C23 H23 0.9500 . ? C24 C25 1.390(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.396(3) . ? C26 C27 1.395(3) . ? C27 C28 1.385(3) . ? C27 H27 0.9500 . ? C28 C29 1.383(4) . ? C28 H28 0.9500 . ? C29 C30 1.388(4) . ? C29 H29 0.9500 . ? C30 C31 1.386(4) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C36 C37 1.519(4) . ? C36 C38 1.530(3) . ? C36 H36 1.0000 . ? 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 1.387(3) . ? C39 C44 1.389(3) . ? C40 C41 1.389(3) . ? C40 H40 0.9500 . ? C41 C42 1.391(4) . ? C41 H41 0.9500 . ? C42 C43 1.378(4) . ? C42 H42 0.9500 . ? C43 C44 1.392(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.388(3) . ? C45 C50 1.397(3) . ? C46 C47 1.391(3) . ? C46 H46 0.9500 . ? C47 C48 1.380(4) . ? C47 H47 0.9500 . ? C48 C49 1.388(4) . ? C48 H48 0.9500 . ? C49 C50 1.384(4) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.393(3) . ? C51 C56 1.399(3) . ? C52 C53 1.385(3) . ? C52 H52 0.9500 . ? C53 C54 1.396(4) . ? C53 H53 0.9500 . ? C54 C55 1.390(3) . ? C54 H54 0.9500 . ? C55 C56 1.379(3) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C62 1.388(3) . ? C57 C58 1.395(3) . ? C58 C59 1.388(3) . ? C58 H58 0.9500 . ? C59 C60 1.383(4) . ? C59 H59 0.9500 . ? C60 C61 1.383(4) . ? C60 H60 0.9500 . ? C61 C62 1.392(3) . ? C61 H61 0.9500 . ? C62 H62 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 C4 Cr1 C3 97.59(12) . . ? C4 Cr1 C1 87.38(11) . . ? C3 Cr1 C1 87.40(11) . . ? C4 Cr1 C2 85.74(11) . . ? C3 Cr1 C2 83.98(12) . . ? C1 Cr1 C2 168.16(11) . . ? C4 Cr1 P2 166.46(9) . . ? C3 Cr1 P2 94.95(9) . . ? C1 Cr1 P2 88.09(8) . . ? C2 Cr1 P2 100.70(9) . . ? C4 Cr1 P1 99.35(9) . . ? C3 Cr1 P1 162.55(9) . . ? C1 Cr1 P1 89.20(8) . . ? C2 Cr1 P1 101.41(8) . . ? P2 Cr1 P1 67.82(4) . . yes C34 Cr2 C35 98.75(12) . . ? C34 Cr2 C33 83.10(11) . . ? C35 Cr2 C33 90.26(11) . . ? C34 Cr2 C32 86.24(11) . . ? C35 Cr2 C32 84.71(11) . . ? C33 Cr2 C32 167.39(11) . . ? C34 Cr2 P4 96.84(8) . . ? C35 Cr2 P4 164.20(9) . . ? C33 Cr2 P4 89.08(8) . . ? C32 Cr2 P4 98.89(8) . . ? C34 Cr2 P3 163.13(8) . . ? C35 Cr2 P3 96.34(9) . . ? C33 Cr2 P3 89.35(8) . . ? C32 Cr2 P3 102.67(8) . . ? P4 Cr2 P3 67.87(3) . . ? N1 P1 C8 106.14(11) . . yes N1 P1 C14 106.09(11) . . yes C8 P1 C14 101.39(12) . . yes N1 P1 Cr1 95.45(8) . . yes C8 P1 Cr1 118.90(8) . . ? C14 P1 Cr1 126.49(9) . . ? N1 P2 C26 104.69(10) . . yes N1 P2 C20 111.73(11) . . yes C26 P2 C20 102.88(11) . . yes N1 P2 Cr1 95.76(8) . . yes C26 P2 Cr1 127.16(9) . . ? C20 P2 Cr1 113.84(8) . . ? N2 P3 C45 109.51(11) . . yes N2 P3 C39 106.41(10) . . yes C45 P3 C39 102.18(11) . . yes N2 P3 Cr2 95.87(7) . . yes C45 P3 Cr2 115.38(8) . . ? C39 P3 Cr2 126.39(8) . . ? N2 P4 C57 107.78(11) . . yes N2 P4 C51 105.85(11) . . yes C57 P4 C51 100.83(11) . . yes N2 P4 Cr2 96.60(7) . . yes C57 P4 Cr2 117.26(8) . . ? C51 P4 Cr2 126.87(8) . . ? C5 N1 P2 131.96(17) . . ? C5 N1 P1 125.10(16) . . ? P2 N1 P1 99.86(11) . . ? C36 N2 P3 132.65(16) . . ? C36 N2 P4 124.82(16) . . ? P3 N2 P4 99.44(11) . . ? O1 C1 Cr1 175.6(2) . . ? O2 C2 Cr1 171.1(2) . . ? O3 C3 Cr1 178.1(2) . . ? O4 C4 Cr1 179.6(3) . . ? N1 C5 C7 112.2(2) . . ? N1 C5 C6 113.8(2) . . ? C7 C5 C6 110.7(2) . . ? N1 C5 H5 106.5 . . ? C7 C5 H5 106.5 . . ? C6 C5 H5 106.5 . . ? 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 . . ? C13 C8 C9 119.4(2) . . ? C13 C8 P1 121.6(2) . . ? C9 C8 P1 118.91(19) . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 120.2(2) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 119.9(3) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C8 C13 C12 120.5(3) . . ? C8 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C19 118.9(2) . . ? C15 C14 P1 120.6(2) . . ? C19 C14 P1 120.4(2) . . ? C16 C15 C14 120.6(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 119.9(3) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.4(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 119.8(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C14 120.5(3) . . ? C18 C19 H19 119.8 . . ? C14 C19 H19 119.8 . . ? C21 C20 C25 118.4(2) . . ? C21 C20 P2 124.62(19) . . ? C25 C20 P2 116.41(18) . . ? C22 C21 C20 120.8(2) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 120.4(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 119.4(2) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 120.4(2) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C20 120.6(2) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? C31 C26 C27 118.3(2) . . ? C31 C26 P2 119.06(19) . . ? C27 C26 P2 122.07(19) . . ? C28 C27 C26 121.1(2) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 120.0(2) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 119.6(2) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C31 C30 C29 120.4(3) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C26 120.5(2) . . ? C30 C31 H31 119.7 . . ? C26 C31 H31 119.7 . . ? O5 C32 Cr2 171.4(2) . . ? O6 C33 Cr2 174.5(2) . . ? O7 C34 Cr2 176.8(2) . . ? O8 C35 Cr2 177.9(2) . . ? N2 C36 C37 112.8(2) . . ? N2 C36 C38 113.5(2) . . ? C37 C36 C38 111.3(2) . . ? N2 C36 H36 106.2 . . ? C37 C36 H36 106.2 . . ? C38 C36 H36 106.2 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 119.3(2) . . ? C40 C39 P3 121.98(18) . . ? C44 C39 P3 118.52(19) . . ? C39 C40 C41 120.6(2) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C40 C41 C42 119.6(2) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C43 C42 C41 120.3(2) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 119.9(2) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C39 C44 C43 120.4(2) . . ? C39 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C46 C45 C50 118.7(2) . . ? C46 C45 P3 123.2(2) . . ? C50 C45 P3 117.78(18) . . ? C45 C46 C47 120.4(2) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C48 C47 C46 120.3(2) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C47 C48 C49 119.8(2) . . ? C47 C48 H48 120.1 . . ? C49 C48 H48 120.1 . . ? C48 C49 C50 119.9(2) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C49 C50 C45 120.7(2) . . ? C49 C50 H50 119.6 . . ? C45 C50 H50 119.6 . . ? C52 C51 C56 118.8(2) . . ? C52 C51 P4 120.55(19) . . ? C56 C51 P4 120.52(18) . . ? C53 C52 C51 120.7(2) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C52 C53 C54 119.8(2) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C55 C54 C53 119.9(2) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C54 C55 C56 120.0(2) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C55 C56 C51 120.7(2) . . ? C55 C56 H56 119.6 . . ? C51 C56 H56 119.6 . . ? C62 C57 C58 119.4(2) . . ? C62 C57 P4 124.15(19) . . ? C58 C57 P4 116.46(18) . . ? C59 C58 C57 120.4(2) . . ? C59 C58 H58 119.8 . . ? C57 C58 H58 119.8 . . ? C60 C59 C58 119.7(2) . . ? C60 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C59 C60 C61 120.3(2) . . ? C59 C60 H60 119.8 . . ? C61 C60 H60 119.8 . . ? C60 C61 C62 120.0(2) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C57 C62 C61 120.1(2) . . ? C57 C62 H62 119.9 . . ? C61 C62 H62 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 C4 Cr1 P1 N1 168.46(11) . . . . ? C3 Cr1 P1 N1 2.5(3) . . . . ? C1 Cr1 P1 N1 81.25(11) . . . . ? C2 Cr1 P1 N1 -104.04(11) . . . . ? P2 Cr1 P1 N1 -7.01(7) . . . . ? C4 Cr1 P1 C8 56.64(13) . . . . ? C3 Cr1 P1 C8 -109.3(3) . . . . ? C1 Cr1 P1 C8 -30.57(13) . . . . ? C2 Cr1 P1 C8 144.14(13) . . . . ? P2 Cr1 P1 C8 -118.83(10) . . . . ? C4 Cr1 P1 C14 -76.90(13) . . . . ? C3 Cr1 P1 C14 117.2(3) . . . . ? C1 Cr1 P1 C14 -164.12(13) . . . . ? C2 Cr1 P1 C14 10.60(13) . . . . ? P2 Cr1 P1 C14 107.62(11) . . . . ? C4 Cr1 P2 N1 -12.4(4) . . . . ? C3 Cr1 P2 N1 -170.12(11) . . . . ? C1 Cr1 P2 N1 -82.89(10) . . . . ? C2 Cr1 P2 N1 105.09(11) . . . . ? P1 Cr1 P2 N1 7.03(7) . . . . ? C4 Cr1 P2 C26 -125.7(4) . . . . ? C3 Cr1 P2 C26 76.55(13) . . . . ? C1 Cr1 P2 C26 163.77(12) . . . . ? C2 Cr1 P2 C26 -8.24(13) . . . . ? P1 Cr1 P2 C26 -106.31(10) . . . . ? C4 Cr1 P2 C20 104.4(4) . . . . ? C3 Cr1 P2 C20 -53.28(12) . . . . ? C1 Cr1 P2 C20 33.94(11) . . . . ? C2 Cr1 P2 C20 -138.07(12) . . . . ? P1 Cr1 P2 C20 123.86(9) . . . . ? C34 Cr2 P3 N2 22.9(3) . . . . ? C35 Cr2 P3 N2 176.27(10) . . . . ? C33 Cr2 P3 N2 86.09(10) . . . . ? C32 Cr2 P3 N2 -97.75(10) . . . . ? P4 Cr2 P3 N2 -3.19(7) . . . . ? C34 Cr2 P3 C45 -91.9(3) . . . . ? C35 Cr2 P3 C45 61.42(12) . . . . ? C33 Cr2 P3 C45 -28.77(12) . . . . ? C32 Cr2 P3 C45 147.39(12) . . . . ? P4 Cr2 P3 C45 -118.05(9) . . . . ? C34 Cr2 P3 C39 138.3(3) . . . . ? C35 Cr2 P3 C39 -68.36(12) . . . . ? C33 Cr2 P3 C39 -158.55(12) . . . . ? C32 Cr2 P3 C39 17.62(13) . . . . ? P4 Cr2 P3 C39 112.18(10) . . . . ? C34 Cr2 P4 N2 -169.41(10) . . . . ? C35 Cr2 P4 N2 1.2(3) . . . . ? C33 Cr2 P4 N2 -86.47(11) . . . . ? C32 Cr2 P4 N2 103.34(11) . . . . ? P3 Cr2 P4 N2 3.20(7) . . . . ? C34 Cr2 P4 C57 -55.49(12) . . . . ? C35 Cr2 P4 C57 115.2(3) . . . . ? C33 Cr2 P4 C57 27.45(12) . . . . ? C32 Cr2 P4 C57 -142.74(12) . . . . ? P3 Cr2 P4 C57 117.11(10) . . . . ? C34 Cr2 P4 C51 75.09(13) . . . . ? C35 Cr2 P4 C51 -114.3(3) . . . . ? C33 Cr2 P4 C51 158.03(12) . . . . ? C32 Cr2 P4 C51 -12.16(13) . . . . ? P3 Cr2 P4 C51 -112.30(10) . . . . ? C26 P2 N1 C5 -38.5(2) . . . . ? C20 P2 N1 C5 72.2(2) . . . . ? Cr1 P2 N1 C5 -169.3(2) . . . . ? C26 P2 N1 P1 121.76(11) . . . . ? C20 P2 N1 P1 -127.60(11) . . . . ? Cr1 P2 N1 P1 -9.08(9) . . . . ? C8 P1 N1 C5 -66.6(2) . . . . ? C14 P1 N1 C5 40.7(2) . . . . ? Cr1 P1 N1 C5 171.15(17) . . . . ? C8 P1 N1 P2 131.26(11) . . . . ? C14 P1 N1 P2 -121.44(12) . . . . ? Cr1 P1 N1 P2 9.05(9) . . . . ? C45 P3 N2 C36 -76.3(2) . . . . ? C39 P3 N2 C36 33.5(2) . . . . ? Cr2 P3 N2 C36 164.2(2) . . . . ? C45 P3 N2 P4 123.65(11) . . . . ? C39 P3 N2 P4 -126.61(11) . . . . ? Cr2 P3 N2 P4 4.08(9) . . . . ? C57 P4 N2 C36 72.2(2) . . . . ? C51 P4 N2 C36 -35.0(2) . . . . ? Cr2 P4 N2 C36 -166.34(17) . . . . ? C57 P4 N2 P3 -125.54(10) . . . . ? C51 P4 N2 P3 127.23(11) . . . . ? Cr2 P4 N2 P3 -4.12(9) . . . . ? P2 N1 C5 C7 -57.4(3) . . . . ? P1 N1 C5 C7 146.60(19) . . . . ? P2 N1 C5 C6 69.3(3) . . . . ? P1 N1 C5 C6 -86.7(3) . . . . ? N1 P1 C8 C13 -22.0(2) . . . . ? C14 P1 C8 C13 -132.6(2) . . . . ? Cr1 P1 C8 C13 83.8(2) . . . . yes N1 P1 C8 C9 162.22(18) . . . . ? C14 P1 C8 C9 51.6(2) . . . . ? Cr1 P1 C8 C9 -92.0(2) . . . . yes C13 C8 C9 C10 0.4(4) . . . . ? P1 C8 C9 C10 176.26(18) . . . . ? C8 C9 C10 C11 -0.2(4) . . . . ? C9 C10 C11 C12 0.1(4) . . . . ? C10 C11 C12 C13 -0.2(4) . . . . ? C9 C8 C13 C12 -0.5(4) . . . . ? P1 C8 C13 C12 -176.25(18) . . . . ? C11 C12 C13 C8 0.4(4) . . . . ? N1 P1 C14 C15 102.8(2) . . . . ? C8 P1 C14 C15 -146.5(2) . . . . ? Cr1 P1 C14 C15 -6.9(3) . . . . yes N1 P1 C14 C19 -73.5(2) . . . . ? C8 P1 C14 C19 37.2(2) . . . . ? Cr1 P1 C14 C19 176.82(17) . . . . yes C19 C14 C15 C16 0.5(4) . . . . ? P1 C14 C15 C16 -175.8(2) . . . . ? C14 C15 C16 C17 0.9(4) . . . . ? C15 C16 C17 C18 -1.4(5) . . . . ? C16 C17 C18 C19 0.4(4) . . . . ? C17 C18 C19 C14 1.1(4) . . . . ? C15 C14 C19 C18 -1.5(4) . . . . ? P1 C14 C19 C18 174.9(2) . . . . ? N1 P2 C20 C21 18.7(2) . . . . ? C26 P2 C20 C21 130.5(2) . . . . ? Cr1 P2 C20 C21 -88.4(2) . . . . yes N1 P2 C20 C25 -170.24(18) . . . . ? C26 P2 C20 C25 -58.5(2) . . . . ? Cr1 P2 C20 C25 82.7(2) . . . . yes C25 C20 C21 C22 2.5(4) . . . . ? P2 C20 C21 C22 173.4(2) . . . . ? C20 C21 C22 C23 -1.6(4) . . . . ? C21 C22 C23 C24 -0.6(4) . . . . ? C22 C23 C24 C25 1.7(4) . . . . ? C23 C24 C25 C20 -0.8(4) . . . . ? C21 C20 C25 C24 -1.3(4) . . . . ? P2 C20 C25 C24 -172.98(19) . . . . ? N1 P2 C26 C31 -80.9(2) . . . . ? C20 P2 C26 C31 162.24(19) . . . . ? Cr1 P2 C26 C31 28.3(2) . . . . yes N1 P2 C26 C27 90.6(2) . . . . ? C20 P2 C26 C27 -26.3(2) . . . . ? Cr1 P2 C26 C27 -160.19(16) . . . . yes C31 C26 C27 C28 1.9(4) . . . . ? P2 C26 C27 C28 -169.62(18) . . . . ? C26 C27 C28 C29 -0.2(4) . . . . ? C27 C28 C29 C30 -1.4(4) . . . . ? C28 C29 C30 C31 1.2(4) . . . . ? C29 C30 C31 C26 0.6(4) . . . . ? C27 C26 C31 C30 -2.1(4) . . . . ? P2 C26 C31 C30 169.7(2) . . . . ? P3 N2 C36 C37 59.2(3) . . . . ? P4 N2 C36 C37 -144.98(18) . . . . ? P3 N2 C36 C38 -68.5(3) . . . . ? P4 N2 C36 C38 87.3(2) . . . . ? N2 P3 C39 C40 -88.3(2) . . . . ? C45 P3 C39 C40 26.6(2) . . . . ? Cr2 P3 C39 C40 161.29(16) . . . . yes N2 P3 C39 C44 86.3(2) . . . . ? C45 P3 C39 C44 -158.9(2) . . . . ? Cr2 P3 C39 C44 -24.1(2) . . . . yes C44 C39 C40 C41 -1.6(4) . . . . ? P3 C39 C40 C41 172.96(19) . . . . ? C39 C40 C41 C42 0.2(4) . . . . ? C40 C41 C42 C43 1.2(4) . . . . ? C41 C42 C43 C44 -1.1(4) . . . . ? C40 C39 C44 C43 1.7(4) . . . . ? P3 C39 C44 C43 -173.1(2) . . . . ? C42 C43 C44 C39 -0.3(4) . . . . ? N2 P3 C45 C46 -18.5(2) . . . . ? C39 P3 C45 C46 -131.0(2) . . . . ? Cr2 P3 C45 C46 88.2(2) . . . . yes N2 P3 C45 C50 167.70(18) . . . . ? C39 P3 C45 C50 55.2(2) . . . . ? Cr2 P3 C45 C50 -85.6(2) . . . . yes C50 C45 C46 C47 -3.1(4) . . . . ? P3 C45 C46 C47 -176.8(2) . . . . ? C45 C46 C47 C48 2.1(4) . . . . ? C46 C47 C48 C49 0.6(4) . . . . ? C47 C48 C49 C50 -2.1(4) . . . . ? C48 C49 C50 C45 1.1(4) . . . . ? C46 C45 C50 C49 1.5(4) . . . . ? P3 C45 C50 C49 175.60(19) . . . . ? N2 P4 C51 C52 -93.2(2) . . . . ? C57 P4 C51 C52 154.6(2) . . . . ? Cr2 P4 C51 C52 18.0(2) . . . . yes N2 P4 C51 C56 83.1(2) . . . . ? C57 P4 C51 C56 -29.1(2) . . . . ? Cr2 P4 C51 C56 -165.67(16) . . . . yes C56 C51 C52 C53 -0.4(4) . . . . ? P4 C51 C52 C53 175.9(2) . . . . ? C51 C52 C53 C54 -0.3(4) . . . . ? C52 C53 C54 C55 0.6(4) . . . . ? C53 C54 C55 C56 -0.1(4) . . . . ? C54 C55 C56 C51 -0.7(4) . . . . ? C52 C51 C56 C55 1.0(4) . . . . ? P4 C51 C56 C55 -175.43(19) . . . . ? N2 P4 C57 C62 1.7(2) . . . . ? C51 P4 C57 C62 112.4(2) . . . . ? Cr2 P4 C57 C62 -105.8(2) . . . . yes N2 P4 C57 C58 -179.56(18) . . . . ? C51 P4 C57 C58 -68.9(2) . . . . ? Cr2 P4 C57 C58 72.9(2) . . . . yes C62 C57 C58 C59 -1.0(4) . . . . ? P4 C57 C58 C59 -179.81(19) . . . . ? C57 C58 C59 C60 0.1(4) . . . . ? C58 C59 C60 C61 0.9(4) . . . . ? C59 C60 C61 C62 -1.0(4) . . . . ? C58 C57 C62 C61 0.9(4) . . . . ? P4 C57 C62 C61 179.6(2) . . . . ? C60 C61 C62 C57 0.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.551 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.081 data_lb050sad _database_code_depnum_ccdc_archive 'CCDC 626713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H31 Cr N O8 P2, C H2 Cl2' _chemical_formula_sum 'C34 H33 Cl2 Cr N O8 P2' _chemical_formula_weight 768.45 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' Cl Cl 0.1484 0.1585 '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' Cr Cr 0.3209 0.6236 '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 10.850(2) _cell_length_b 13.509(3) _cell_length_c 13.657(3) _cell_angle_alpha 76.40(3) _cell_angle_beta 67.08(3) _cell_angle_gamma 81.53(3) _cell_volume 1788.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5728 _cell_measurement_theta_min 2.334 _cell_measurement_theta_max 27.538 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.674724 _exptl_absorpt_correction_T_max 0.960000 _exptl_absorpt_process_details 'SADABS V2.1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18942 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.65 _reflns_number_total 8213 _reflns_number_gt 5541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _computing_publication_material 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+1.0650P] 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 8213 _refine_ls_number_parameters 438 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1373 _refine_ls_wR_factor_gt 0.1203 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _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 Cr1 Cr 0.82371(4) 0.28630(3) 0.20891(4) 0.02229(13) Uani 1 1 d . . . Cl1 Cl 0.47960(17) 0.65004(16) 0.15713(14) 0.1355(8) Uani 1 1 d . . . Cl2 Cl 0.56435(15) 0.84946(14) 0.04373(15) 0.1068(5) Uani 1 1 d . . . P1 P 0.93515(7) 0.31406(5) 0.31777(6) 0.02153(16) Uani 1 1 d . . . P2 P 0.85882(7) 0.13403(5) 0.32359(6) 0.02255(17) Uani 1 1 d . . . N1 N 0.9413(2) 0.18863(17) 0.37935(18) 0.0226(5) Uani 1 1 d . . . O1 O 0.5347(2) 0.32181(18) 0.35825(19) 0.0402(6) Uani 1 1 d . . . O2 O 1.0853(2) 0.23225(19) 0.03453(18) 0.0451(6) Uani 1 1 d . . . O3 O 0.8188(3) 0.50565(19) 0.0932(2) 0.0570(7) Uani 1 1 d . . . O4 O 0.6960(2) 0.2140(2) 0.0804(2) 0.0499(7) Uani 1 1 d . . . O5 O 1.0211(2) 0.33553(15) 0.49816(16) 0.0304(5) Uani 1 1 d . . . O6 O 1.0247(2) 0.51505(15) 0.20624(17) 0.0347(5) Uani 1 1 d . . . O7 O 0.6552(2) 0.20128(16) 0.51918(17) 0.0375(5) Uani 1 1 d . . . O8 O 0.8195(2) 0.00792(17) 0.19339(18) 0.0381(5) Uani 1 1 d . . . C1 C 0.9620(3) 0.1426(2) 0.4809(2) 0.0311(7) Uani 1 1 d . . . H1A H 0.9011 0.1759 0.5379 0.047 Uiso 1 1 calc R . . H1B H 1.0525 0.1504 0.4719 0.047 Uiso 1 1 calc R . . H1C H 0.9459 0.0713 0.4993 0.047 Uiso 1 1 calc R . . C2 C 0.6466(3) 0.3087(2) 0.3063(2) 0.0275(6) Uani 1 1 d . . . C3 C 0.9885(3) 0.2547(2) 0.1027(2) 0.0277(6) Uani 1 1 d . . . C4 C 0.8207(3) 0.4222(2) 0.1374(3) 0.0336(7) Uani 1 1 d . . . C5 C 0.7448(3) 0.2401(2) 0.1309(2) 0.0310(7) Uani 1 1 d . . . C6 C 0.8562(3) 0.3926(2) 0.4218(2) 0.0246(6) Uani 1 1 d . . . C7 C 0.9038(3) 0.3920(2) 0.5046(2) 0.0274(6) Uani 1 1 d . . . C8 C 0.8334(3) 0.4480(2) 0.5853(2) 0.0330(7) Uani 1 1 d . . . H8 H 0.8626 0.4445 0.6417 0.040 Uiso 1 1 calc R . . C9 C 0.7204(3) 0.5088(2) 0.5819(3) 0.0356(7) Uani 1 1 d . . . H9 H 0.6737 0.5459 0.6362 0.043 Uiso 1 1 calc R . . C10 C 0.6760(3) 0.5150(2) 0.4978(3) 0.0354(7) Uani 1 1 d . . . H10 H 0.6019 0.5578 0.4940 0.043 Uiso 1 1 calc R . . C11 C 0.7443(3) 0.4561(2) 0.4192(2) 0.0293(6) Uani 1 1 d . . . H11 H 0.7140 0.4595 0.3634 0.035 Uiso 1 1 calc R . . C12 C 1.0572(4) 0.3150(3) 0.5917(3) 0.0396(8) Uani 1 1 d . . . H12A H 1.0713 0.3780 0.6056 0.059 Uiso 1 1 calc R . . H12B H 1.1381 0.2717 0.5789 0.059 Uiso 1 1 calc R . . H12C H 0.9864 0.2816 0.6532 0.059 Uiso 1 1 calc R . . C13 C 1.1095(3) 0.3499(2) 0.2548(2) 0.0245(6) Uani 1 1 d . . . C14 C 1.1360(3) 0.4501(2) 0.1989(2) 0.0287(6) Uani 1 1 d . . . C15 C 1.2683(3) 0.4791(3) 0.1423(2) 0.0368(8) Uani 1 1 d . . . H15 H 1.2855 0.5455 0.1044 0.044 Uiso 1 1 calc R . . C16 C 1.3726(3) 0.4072(3) 0.1437(3) 0.0423(8) Uani 1 1 d . . . H16 H 1.4605 0.4262 0.1074 0.051 Uiso 1 1 calc R . . C17 C 1.3490(3) 0.3082(3) 0.1979(3) 0.0422(8) Uani 1 1 d . . . H17 H 1.4204 0.2608 0.1979 0.051 Uiso 1 1 calc R . . C18 C 1.2177(3) 0.2792(2) 0.2529(3) 0.0325(7) Uani 1 1 d . . . H18 H 1.2020 0.2120 0.2887 0.039 Uiso 1 1 calc R . . C19 C 1.0423(4) 0.6162(2) 0.1448(3) 0.0463(9) Uani 1 1 d . . . H19A H 1.0947 0.6506 0.1676 0.069 Uiso 1 1 calc R . . H19B H 0.9563 0.6523 0.1559 0.069 Uiso 1 1 calc R . . H19C H 1.0877 0.6140 0.0693 0.069 Uiso 1 1 calc R . . C20 C 0.7384(3) 0.0550(2) 0.4414(2) 0.0277(6) Uani 1 1 d . . . C21 C 0.6477(3) 0.0992(2) 0.5284(2) 0.0314(7) Uani 1 1 d . . . C22 C 0.5575(3) 0.0393(3) 0.6182(3) 0.0414(8) Uani 1 1 d . . . H22 H 0.4980 0.0689 0.6755 0.050 Uiso 1 1 calc R . . C23 C 0.5563(3) -0.0630(3) 0.6223(3) 0.0433(8) Uani 1 1 d . . . H23 H 0.4950 -0.1022 0.6820 0.052 Uiso 1 1 calc R . . C24 C 0.6454(3) -0.1084(3) 0.5388(3) 0.0409(8) Uani 1 1 d . . . H24 H 0.6448 -0.1779 0.5422 0.049 Uiso 1 1 calc R . . C25 C 0.7356(3) -0.0494(2) 0.4498(2) 0.0305(7) Uani 1 1 d . . . H25 H 0.7960 -0.0804 0.3940 0.037 Uiso 1 1 calc R . . C26 C 0.5678(4) 0.2483(3) 0.6080(3) 0.0585(11) Uani 1 1 d . . . H26A H 0.4762 0.2415 0.6190 0.088 Uiso 1 1 calc R . . H26B H 0.5844 0.3193 0.5918 0.088 Uiso 1 1 calc R . . H26C H 0.5843 0.2154 0.6725 0.088 Uiso 1 1 calc R . . C27 C 0.9784(3) 0.0358(2) 0.2589(2) 0.0260(6) Uani 1 1 d . . . C28 C 0.9451(3) -0.0169(2) 0.1958(2) 0.0306(7) Uani 1 1 d . . . C29 C 1.0374(4) -0.0884(2) 0.1415(3) 0.0392(8) Uani 1 1 d . . . H29 H 1.0148 -0.1235 0.1005 0.047 Uiso 1 1 calc R . . C30 C 1.1618(4) -0.1063(3) 0.1491(3) 0.0448(9) Uani 1 1 d . . . H30 H 1.2231 -0.1535 0.1125 0.054 Uiso 1 1 calc R . . C31 C 1.1974(3) -0.0560(3) 0.2098(3) 0.0398(8) Uani 1 1 d . . . H31 H 1.2817 -0.0694 0.2144 0.048 Uiso 1 1 calc R . . C32 C 1.1056(3) 0.0158(2) 0.2646(2) 0.0326(7) Uani 1 1 d . . . H32 H 1.1297 0.0504 0.3051 0.039 Uiso 1 1 calc R . . C33 C 0.7743(4) -0.0462(3) 0.1358(3) 0.0469(9) Uani 1 1 d . . . H33A H 0.8370 -0.0406 0.0624 0.070 Uiso 1 1 calc R . . H33B H 0.6879 -0.0174 0.1360 0.070 Uiso 1 1 calc R . . H33C H 0.7678 -0.1169 0.1707 0.070 Uiso 1 1 calc R . . C34 C 0.6138(5) 0.7179(4) 0.0718(4) 0.0931(19) Uani 1 1 d . . . H34A H 0.6538 0.6925 0.0047 0.112 Uiso 1 1 calc R . . H34B H 0.6805 0.7091 0.1045 0.112 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 Cr1 0.0234(2) 0.0247(2) 0.0186(2) -0.00654(18) -0.00719(19) 0.00113(18) Cl1 0.1099(12) 0.1769(18) 0.1038(12) -0.0718(12) 0.0326(10) -0.0934(13) Cl2 0.0769(10) 0.1225(13) 0.1347(14) -0.0525(11) -0.0385(10) -0.0047(9) P1 0.0235(4) 0.0217(4) 0.0191(3) -0.0057(3) -0.0069(3) -0.0002(3) P2 0.0231(4) 0.0233(4) 0.0199(4) -0.0058(3) -0.0057(3) -0.0009(3) N1 0.0257(12) 0.0219(11) 0.0216(12) -0.0057(10) -0.0097(10) -0.0005(9) O1 0.0271(12) 0.0468(14) 0.0449(14) -0.0201(12) -0.0074(11) 0.0048(10) O2 0.0349(13) 0.0540(15) 0.0309(12) -0.0076(11) 0.0010(11) 0.0054(11) O3 0.091(2) 0.0316(14) 0.0574(17) 0.0030(12) -0.0442(16) -0.0017(13) O4 0.0485(15) 0.0698(18) 0.0482(15) -0.0285(14) -0.0273(13) -0.0003(13) O5 0.0354(12) 0.0340(11) 0.0271(11) -0.0110(9) -0.0162(9) 0.0033(9) O6 0.0404(13) 0.0260(11) 0.0315(12) 0.0015(9) -0.0105(10) -0.0025(9) O7 0.0375(13) 0.0350(12) 0.0256(11) -0.0067(10) 0.0024(10) 0.0029(10) O8 0.0449(14) 0.0391(13) 0.0385(13) -0.0168(11) -0.0182(11) -0.0044(10) C1 0.0402(18) 0.0272(15) 0.0307(16) -0.0047(13) -0.0198(14) 0.0013(13) C2 0.0318(17) 0.0257(15) 0.0284(15) -0.0098(13) -0.0137(14) 0.0023(12) C3 0.0289(16) 0.0274(15) 0.0248(15) -0.0016(12) -0.0106(13) 0.0005(12) C4 0.0395(19) 0.0354(18) 0.0292(17) -0.0089(14) -0.0161(14) 0.0016(14) C5 0.0261(16) 0.0357(17) 0.0297(16) -0.0112(14) -0.0074(13) 0.0020(13) C6 0.0258(15) 0.0245(14) 0.0216(14) -0.0055(12) -0.0061(12) -0.0018(11) C7 0.0274(16) 0.0276(15) 0.0259(15) -0.0061(12) -0.0076(12) -0.0030(12) C8 0.0388(18) 0.0356(17) 0.0251(16) -0.0126(14) -0.0085(14) -0.0022(14) C9 0.0373(18) 0.0366(17) 0.0317(17) -0.0181(14) -0.0062(14) 0.0010(14) C10 0.0302(17) 0.0332(17) 0.0427(19) -0.0164(15) -0.0106(15) 0.0053(13) C11 0.0299(16) 0.0302(15) 0.0309(16) -0.0106(13) -0.0121(13) -0.0011(12) C12 0.051(2) 0.0417(19) 0.0333(18) -0.0063(15) -0.0264(16) 0.0029(16) C13 0.0278(15) 0.0284(15) 0.0189(14) -0.0073(12) -0.0078(12) -0.0046(12) C14 0.0340(17) 0.0333(16) 0.0205(14) -0.0087(13) -0.0092(13) -0.0043(13) C15 0.0422(19) 0.0398(18) 0.0267(16) -0.0070(14) -0.0062(14) -0.0154(15) C16 0.0301(18) 0.057(2) 0.0354(18) -0.0106(17) -0.0021(15) -0.0149(16) C17 0.0274(18) 0.051(2) 0.044(2) -0.0109(17) -0.0082(16) -0.0022(15) C18 0.0293(17) 0.0342(17) 0.0332(17) -0.0083(14) -0.0096(14) -0.0017(13) C19 0.072(3) 0.0300(17) 0.0294(18) 0.0019(14) -0.0155(18) -0.0028(17) C20 0.0233(15) 0.0337(16) 0.0237(15) -0.0017(13) -0.0076(12) -0.0039(12) C21 0.0256(16) 0.0349(17) 0.0264(16) -0.0007(13) -0.0053(13) 0.0000(13) C22 0.0295(18) 0.051(2) 0.0292(17) 0.0017(15) -0.0016(14) 0.0013(15) C23 0.0313(18) 0.048(2) 0.0369(19) 0.0101(16) -0.0054(15) -0.0101(15) C24 0.0366(19) 0.0369(18) 0.046(2) 0.0022(16) -0.0142(16) -0.0119(15) C25 0.0300(16) 0.0317(16) 0.0305(16) -0.0025(13) -0.0122(13) -0.0066(13) C26 0.064(3) 0.049(2) 0.035(2) -0.0122(18) 0.0096(19) 0.0081(19) C27 0.0289(16) 0.0208(14) 0.0226(14) -0.0048(12) -0.0031(12) -0.0013(11) C28 0.0391(18) 0.0262(15) 0.0237(15) -0.0043(12) -0.0081(14) -0.0043(13) C29 0.054(2) 0.0296(17) 0.0302(17) -0.0124(14) -0.0071(16) -0.0034(15) C30 0.052(2) 0.0352(18) 0.0333(18) -0.0124(15) -0.0013(17) 0.0062(16) C31 0.0352(19) 0.0382(18) 0.0365(19) -0.0085(15) -0.0061(15) 0.0081(14) C32 0.0361(18) 0.0287(16) 0.0290(16) -0.0052(13) -0.0091(14) 0.0011(13) C33 0.059(2) 0.050(2) 0.038(2) -0.0140(17) -0.0159(18) -0.0186(18) C34 0.077(4) 0.105(4) 0.083(4) -0.050(3) 0.016(3) -0.037(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 Cr1 C5 1.853(3) . yes Cr1 C4 1.868(3) . yes Cr1 C3 1.879(3) . yes Cr1 C2 1.892(3) . yes Cr1 P2 2.3556(12) . yes Cr1 P1 2.3683(10) . yes Cl1 C34 1.699(5) . ? Cl2 C34 1.775(6) . ? P1 N1 1.710(2) . yes P1 C13 1.833(3) . yes P1 C6 1.836(3) . yes P2 N1 1.707(2) . yes P2 C27 1.837(3) . yes P2 C20 1.844(3) . yes N1 C1 1.468(4) . yes O1 C2 1.154(3) . ? O2 C3 1.158(3) . ? O3 C4 1.148(4) . ? O4 C5 1.156(4) . ? O5 C7 1.366(3) . ? O5 C12 1.433(3) . ? O6 C14 1.368(4) . ? O6 C19 1.421(4) . ? O7 C21 1.366(4) . ? O7 C26 1.436(4) . ? O8 C28 1.366(4) . ? O8 C33 1.439(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C6 C11 1.387(4) . ? C6 C7 1.412(4) . ? C7 C8 1.392(4) . ? C8 C9 1.383(4) . ? C8 H8 0.9300 . ? C9 C10 1.390(4) . ? C9 H9 0.9300 . ? C10 C11 1.393(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.399(4) . ? C13 C18 1.396(4) . ? C14 C15 1.404(4) . ? C15 C16 1.381(5) . ? C15 H15 0.9300 . ? C16 C17 1.375(5) . ? C16 H16 0.9300 . ? C17 C18 1.392(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C25 1.392(4) . ? C20 C21 1.409(4) . ? C21 C22 1.396(4) . ? C22 C23 1.371(5) . ? C22 H22 0.9300 . ? C23 C24 1.381(5) . ? C23 H23 0.9300 . ? C24 C25 1.385(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C32 1.395(4) . ? C27 C28 1.410(4) . ? C28 C29 1.400(4) . ? C29 C30 1.376(5) . ? C29 H29 0.9300 . ? C30 C31 1.374(5) . ? C30 H30 0.9300 . ? C31 C32 1.403(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9700 . ? C34 H34B 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 C5 Cr1 C4 94.68(14) . . ? C5 Cr1 C3 86.18(13) . . ? C4 Cr1 C3 92.15(14) . . ? C5 Cr1 C2 85.73(12) . . ? C4 Cr1 C2 89.73(14) . . ? C3 Cr1 C2 171.82(12) . . ? C5 Cr1 P2 101.65(10) . . ? C4 Cr1 P2 163.65(10) . . ? C3 Cr1 P2 88.15(10) . . ? C2 Cr1 P2 92.29(10) . . ? C5 Cr1 P1 169.74(10) . . ? C4 Cr1 P1 95.21(10) . . ? C3 Cr1 P1 90.73(9) . . ? C2 Cr1 P1 97.03(9) . . ? P2 Cr1 P1 68.44(3) . . yes N1 P1 C13 105.71(13) . . yes N1 P1 C6 109.27(12) . . yes C13 P1 C6 104.00(13) . . yes N1 P1 Cr1 94.46(8) . . yes C13 P1 Cr1 119.90(9) . . ? C6 P1 Cr1 121.70(10) . . ? N1 P2 C27 105.50(13) . . yes N1 P2 C20 103.84(12) . . yes C27 P2 C20 101.34(14) . . yes N1 P2 Cr1 94.98(8) . . yes C27 P2 Cr1 117.12(10) . . ? C20 P2 Cr1 130.54(10) . . ? C1 N1 P2 124.48(19) . . ? C1 N1 P1 129.82(18) . . ? P2 N1 P1 102.05(12) . . yes C7 O5 C12 117.3(2) . . ? C14 O6 C19 118.4(3) . . ? C21 O7 C26 117.9(3) . . ? C28 O8 C33 118.5(2) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 Cr1 173.7(2) . . ? O2 C3 Cr1 175.5(3) . . ? O3 C4 Cr1 179.8(3) . . ? O4 C5 Cr1 178.1(3) . . ? C11 C6 C7 118.1(2) . . ? C11 C6 P1 118.6(2) . . ? C7 C6 P1 123.3(2) . . ? O5 C7 C8 123.9(3) . . ? O5 C7 C6 116.0(2) . . ? C8 C7 C6 120.2(3) . . ? C9 C8 C7 120.3(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 120.5(3) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.0(3) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C6 C11 C10 121.9(3) . . ? C6 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? O5 C12 H12A 109.5 . . ? O5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 118.5(3) . . ? C14 C13 P1 118.8(2) . . ? C18 C13 P1 122.6(2) . . ? O6 C14 C13 114.9(3) . . ? O6 C14 C15 124.3(3) . . ? C13 C14 C15 120.8(3) . . ? C16 C15 C14 119.0(3) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 121.3(3) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C18 119.8(3) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C18 C13 120.8(3) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? O6 C19 H19A 109.5 . . ? O6 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O6 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 117.7(3) . . ? C25 C20 P2 122.1(2) . . ? C21 C20 P2 120.2(2) . . ? O7 C21 C22 123.4(3) . . ? O7 C21 C20 116.3(3) . . ? C22 C21 C20 120.3(3) . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.6(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 119.4(3) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C20 121.8(3) . . ? C24 C25 H25 119.1 . . ? C20 C25 H25 119.1 . . ? O7 C26 H26A 109.5 . . ? O7 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O7 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 118.4(3) . . ? C32 C27 P2 121.9(2) . . ? C28 C27 P2 119.6(2) . . ? O8 C28 C29 124.8(3) . . ? O8 C28 C27 114.7(2) . . ? C29 C28 C27 120.5(3) . . ? C30 C29 C28 119.5(3) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C31 C30 C29 121.4(3) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 119.5(3) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C27 C32 C31 120.7(3) . . ? C27 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? O8 C33 H33A 109.5 . . ? O8 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O8 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Cl1 C34 Cl2 110.6(3) . . ? Cl1 C34 H34A 109.5 . . ? Cl2 C34 H34A 109.5 . . ? Cl1 C34 H34B 109.5 . . ? Cl2 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? 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 C5 Cr1 P1 N1 -13.7(5) . . . . ? C4 Cr1 P1 N1 -178.30(13) . . . . ? C3 Cr1 P1 N1 -86.08(12) . . . . ? C2 Cr1 P1 N1 91.33(12) . . . . ? P2 Cr1 P1 N1 1.63(8) . . . . ? C5 Cr1 P1 C13 97.2(5) . . . . ? C4 Cr1 P1 C13 -67.32(15) . . . . ? C3 Cr1 P1 C13 24.90(14) . . . . ? C2 Cr1 P1 C13 -157.69(14) . . . . ? P2 Cr1 P1 C13 112.62(12) . . . . ? C5 Cr1 P1 C6 -129.7(5) . . . . ? C4 Cr1 P1 C6 65.77(15) . . . . ? C3 Cr1 P1 C6 157.99(14) . . . . ? C2 Cr1 P1 C6 -24.60(14) . . . . ? P2 Cr1 P1 C6 -114.29(12) . . . . ? C5 Cr1 P2 N1 175.60(12) . . . . ? C4 Cr1 P2 N1 -1.4(4) . . . . ? C3 Cr1 P2 N1 89.88(12) . . . . ? C2 Cr1 P2 N1 -98.29(12) . . . . ? P1 Cr1 P2 N1 -1.64(8) . . . . ? C5 Cr1 P2 C27 65.35(14) . . . . ? C4 Cr1 P2 C27 -111.7(4) . . . . ? C3 Cr1 P2 C27 -20.36(14) . . . . ? C2 Cr1 P2 C27 151.46(14) . . . . ? P1 Cr1 P2 C27 -111.88(11) . . . . ? C5 Cr1 P2 C20 -71.41(16) . . . . ? C4 Cr1 P2 C20 111.6(4) . . . . ? C3 Cr1 P2 C20 -157.13(15) . . . . ? C2 Cr1 P2 C20 14.70(15) . . . . ? P1 Cr1 P2 C20 111.35(13) . . . . ? C27 P2 N1 C1 -77.7(2) . . . . ? C20 P2 N1 C1 28.5(3) . . . . ? Cr1 P2 N1 C1 162.4(2) . . . . ? C27 P2 N1 P1 122.09(13) . . . . ? C20 P2 N1 P1 -131.74(13) . . . . ? Cr1 P2 N1 P1 2.16(10) . . . . ? C13 P1 N1 C1 76.4(3) . . . . ? C6 P1 N1 C1 -35.0(3) . . . . ? Cr1 P1 N1 C1 -160.9(2) . . . . ? C13 P1 N1 P2 -124.92(12) . . . . ? C6 P1 N1 P2 123.70(13) . . . . ? Cr1 P1 N1 P2 -2.14(10) . . . . ? C5 Cr1 C2 O1 -18(2) . . . . ? C4 Cr1 C2 O1 77(2) . . . . ? C3 Cr1 C2 O1 -26(3) . . . . ? P2 Cr1 C2 O1 -119(2) . . . . ? P1 Cr1 C2 O1 172(2) . . . . ? C5 Cr1 C3 O2 -7(3) . . . . ? C4 Cr1 C3 O2 -102(3) . . . . ? C2 Cr1 C3 O2 1(4) . . . . ? P2 Cr1 C3 O2 95(3) . . . . ? P1 Cr1 C3 O2 163(3) . . . . ? C5 Cr1 C4 O3 -29(100) . . . . ? C3 Cr1 C4 O3 57(100) . . . . ? C2 Cr1 C4 O3 -115(100) . . . . ? P2 Cr1 C4 O3 148(100) . . . . ? P1 Cr1 C4 O3 148(100) . . . . ? C4 Cr1 C5 O4 9(8) . . . . ? C3 Cr1 C5 O4 -83(8) . . . . ? C2 Cr1 C5 O4 98(8) . . . . ? P2 Cr1 C5 O4 -170(8) . . . . ? P1 Cr1 C5 O4 -156(8) . . . . ? N1 P1 C6 C11 -123.8(2) . . . . ? C13 P1 C6 C11 123.7(2) . . . . ? Cr1 P1 C6 C11 -15.6(3) . . . . ? N1 P1 C6 C7 56.4(3) . . . . ? C13 P1 C6 C7 -56.1(3) . . . . ? Cr1 P1 C6 C7 164.6(2) . . . . yes C12 O5 C7 C8 14.2(4) . . . . ? C12 O5 C7 C6 -166.9(3) . . . . ? C11 C6 C7 O5 -174.2(3) . . . . ? P1 C6 C7 O5 5.6(4) . . . . ? C11 C6 C7 C8 4.7(4) . . . . ? P1 C6 C7 C8 -175.4(2) . . . . ? O5 C7 C8 C9 175.5(3) . . . . ? C6 C7 C8 C9 -3.4(5) . . . . ? C7 C8 C9 C10 -0.2(5) . . . . ? C8 C9 C10 C11 2.3(5) . . . . ? C7 C6 C11 C10 -2.6(4) . . . . ? P1 C6 C11 C10 177.5(2) . . . . ? C9 C10 C11 C6 -0.9(5) . . . . ? N1 P1 C13 C14 -179.1(2) . . . . ? C6 P1 C13 C14 -64.1(2) . . . . ? Cr1 P1 C13 C14 76.1(2) . . . . yes N1 P1 C13 C18 6.1(3) . . . . ? C6 P1 C13 C18 121.2(2) . . . . ? Cr1 P1 C13 C18 -98.6(2) . . . . ? C19 O6 C14 C13 -175.0(2) . . . . ? C19 O6 C14 C15 6.1(4) . . . . ? C18 C13 C14 O6 -178.9(2) . . . . ? P1 C13 C14 O6 6.1(3) . . . . ? C18 C13 C14 C15 -0.1(4) . . . . ? P1 C13 C14 C15 -175.0(2) . . . . ? O6 C14 C15 C16 177.9(3) . . . . ? C13 C14 C15 C16 -0.9(4) . . . . ? C14 C15 C16 C17 1.1(5) . . . . ? C15 C16 C17 C18 -0.2(5) . . . . ? C16 C17 C18 C13 -0.8(5) . . . . ? C14 C13 C18 C17 0.9(4) . . . . ? P1 C13 C18 C17 175.7(2) . . . . ? N1 P2 C20 C25 -123.2(2) . . . . ? C27 P2 C20 C25 -13.9(3) . . . . ? Cr1 P2 C20 C25 127.7(2) . . . . ? N1 P2 C20 C21 54.9(3) . . . . ? C27 P2 C20 C21 164.2(2) . . . . ? Cr1 P2 C20 C21 -54.2(3) . . . . yes C26 O7 C21 C22 1.5(5) . . . . ? C26 O7 C21 C20 -177.8(3) . . . . ? C25 C20 C21 O7 178.2(3) . . . . ? P2 C20 C21 O7 0.1(4) . . . . ? C25 C20 C21 C22 -1.0(4) . . . . ? P2 C20 C21 C22 -179.2(2) . . . . ? O7 C21 C22 C23 -179.4(3) . . . . ? C20 C21 C22 C23 -0.2(5) . . . . ? C21 C22 C23 C24 1.0(5) . . . . ? C22 C23 C24 C25 -0.6(5) . . . . ? C23 C24 C25 C20 -0.6(5) . . . . ? C21 C20 C25 C24 1.5(4) . . . . ? P2 C20 C25 C24 179.6(2) . . . . ? N1 P2 C27 C32 2.1(3) . . . . ? C20 P2 C27 C32 -105.9(3) . . . . ? Cr1 P2 C27 C32 106.2(2) . . . . ? N1 P2 C27 C28 -173.7(2) . . . . ? C20 P2 C27 C28 78.3(3) . . . . ? Cr1 P2 C27 C28 -69.6(2) . . . . yes C33 O8 C28 C29 3.4(5) . . . . ? C33 O8 C28 C27 -176.6(3) . . . . ? C32 C27 C28 O8 -179.2(3) . . . . ? P2 C27 C28 O8 -3.2(4) . . . . ? C32 C27 C28 C29 0.8(4) . . . . ? P2 C27 C28 C29 176.8(2) . . . . ? O8 C28 C29 C30 179.4(3) . . . . ? C27 C28 C29 C30 -0.6(5) . . . . ? C28 C29 C30 C31 0.4(5) . . . . ? C29 C30 C31 C32 -0.4(5) . . . . ? C28 C27 C32 C31 -0.8(5) . . . . ? P2 C27 C32 C31 -176.7(2) . . . . ? C30 C31 C32 C27 0.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.211 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.074 data_lb106sadsqueeze _database_code_depnum_ccdc_archive 'CCDC 626714' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H31 Cr N2 O8 P2, B F4' _chemical_formula_sum 'C32 H31 B Cr F4 N2 O8 P2' _chemical_formula_weight 772.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 11.398(2) _cell_length_b 19.022(4) _cell_length_c 18.460(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.33(3) _cell_angle_gamma 90.00 _cell_volume 3924.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3331 _cell_measurement_theta_min 3.371 _cell_measurement_theta_max 79.553 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 3.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.538660 _exptl_absorpt_correction_T_max 0.890000 _exptl_absorpt_process_details 'SADABS V2.10' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29906 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.0925 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 70.07 _reflns_number_total 7312 _reflns_number_gt 4672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _computing_publication_material 'Bruker SHELXTL V6.1 (Bruker AXS, 2000)' _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. ; # SQUEEZE RESULTS 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 1 -0.018 0.000 0.000 317.0 83.3 2 0.004 0.500 0.500 317.0 83.2 _platon_squeeze_details ; ? ; _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^)+(0.0466P)^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 7312 _refine_ls_number_parameters 502 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 Cr1 Cr 0.26821(4) 0.44672(2) 0.07496(3) 0.03265(15) Uani 1 1 d . . . P1 P 0.33076(7) 0.43560(4) 0.20807(5) 0.0348(2) Uani 1 1 d . . . P2 P 0.27933(7) 0.55735(3) 0.13634(4) 0.03211(19) Uani 1 1 d . . . N1 N 0.3275(2) 0.52387(11) 0.22200(13) 0.0336(6) Uani 1 1 d . . . N2 N 0.2394(2) 0.47331(13) -0.01898(19) 0.0449(7) Uani 1 1 d . . . O1 O 0.2241(2) 0.48938(11) -0.08097(14) 0.0450(6) Uani 1 1 d . . . O2 O 0.2570(2) 0.29310(11) 0.04046(13) 0.0504(6) Uani 1 1 d . . . O3 O -0.0039(2) 0.43525(11) 0.06246(14) 0.0483(6) Uani 1 1 d . . . O4 O 0.5354(2) 0.46295(11) 0.07529(13) 0.0438(6) Uani 1 1 d . . . O5 O 0.1313(2) 0.32957(11) 0.17762(17) 0.0610(7) Uani 1 1 d . . . O6 O 0.4157(2) 0.29894(10) 0.19342(12) 0.0464(6) Uani 1 1 d . . . O7 O 0.06697(18) 0.52183(10) 0.19950(12) 0.0383(5) Uani 1 1 d . . . O8 O 0.28614(18) 0.62562(9) -0.00076(12) 0.0381(5) Uani 1 1 d . . . C1 C 0.3274(3) 0.56331(15) 0.29051(18) 0.0423(8) Uani 1 1 d . . . H1A H 0.2609 0.5485 0.3116 0.064 Uiso 1 1 calc R . . H1B H 0.3207 0.6127 0.2797 0.064 Uiso 1 1 calc R . . H1C H 0.4007 0.5545 0.3250 0.064 Uiso 1 1 calc R . . C2 C 0.0973(3) 0.44077(14) 0.07277(18) 0.0391(8) Uani 1 1 d . . . C3 C 0.4371(3) 0.45592(14) 0.07620(17) 0.0353(7) Uani 1 1 d . . . C4 C 0.2658(3) 0.35201(15) 0.05446(17) 0.0364(7) Uani 1 1 d . . . C5 C 0.2538(3) 0.39264(15) 0.2727(2) 0.0458(9) Uani 1 1 d . . . C6 C 0.1606(3) 0.34375(17) 0.2505(3) 0.0566(11) Uani 1 1 d . . . C7 C 0.1038(4) 0.3141(2) 0.3039(3) 0.0752(14) Uani 1 1 d . . . H7 H 0.0413 0.2824 0.2898 0.090 Uiso 1 1 calc R . . C8 C 0.1406(5) 0.3318(2) 0.3777(4) 0.0923(18) Uani 1 1 d . . . H8 H 0.1011 0.3123 0.4124 0.111 Uiso 1 1 calc R . . C9 C 0.2344(4) 0.3779(2) 0.4012(3) 0.0770(14) Uani 1 1 d . . . H9 H 0.2583 0.3892 0.4509 0.092 Uiso 1 1 calc R . . C10 C 0.2919(4) 0.40661(18) 0.3484(2) 0.0575(10) Uani 1 1 d . . . H10 H 0.3574 0.4359 0.3636 0.069 Uiso 1 1 calc R . . C11 C 0.0454(4) 0.27458(18) 0.1547(3) 0.0893(17) Uani 1 1 d . . . H11A H 0.0752 0.2312 0.1779 0.134 Uiso 1 1 calc R . . H11B H 0.0324 0.2694 0.1020 0.134 Uiso 1 1 calc R . . H11C H -0.0287 0.2864 0.1690 0.134 Uiso 1 1 calc R . . C12 C 0.4846(3) 0.40796(14) 0.24029(16) 0.0357(7) Uani 1 1 d . . . C13 C 0.5126(3) 0.33777(15) 0.22601(17) 0.0387(8) Uani 1 1 d . . . C14 C 0.6284(3) 0.31341(17) 0.24294(18) 0.0458(9) Uani 1 1 d . . . H14 H 0.6462 0.2671 0.2331 0.055 Uiso 1 1 calc R . . C15 C 0.7181(3) 0.35942(19) 0.2751(2) 0.0511(9) Uani 1 1 d . . . H15 H 0.7965 0.3432 0.2869 0.061 Uiso 1 1 calc R . . C16 C 0.6943(3) 0.42867(19) 0.2901(2) 0.0503(9) Uani 1 1 d . . . H16 H 0.7556 0.4586 0.3120 0.060 Uiso 1 1 calc R . . C17 C 0.5769(3) 0.45280(16) 0.27192(18) 0.0411(8) Uani 1 1 d . . . H17 H 0.5600 0.4994 0.2810 0.049 Uiso 1 1 calc R . . C18 C 0.4351(4) 0.22785(15) 0.1729(2) 0.0618(12) Uani 1 1 d . . . H18A H 0.4906 0.2273 0.1399 0.093 Uiso 1 1 calc R . . H18B H 0.3605 0.2076 0.1486 0.093 Uiso 1 1 calc R . . H18C H 0.4672 0.2010 0.2163 0.093 Uiso 1 1 calc R . . C19 C 0.1505(3) 0.61260(14) 0.13935(17) 0.0330(7) Uani 1 1 d . . . C20 C 0.0524(3) 0.58656(14) 0.16716(17) 0.0344(7) Uani 1 1 d . . . C21 C -0.0518(3) 0.62614(14) 0.16187(17) 0.0364(7) Uani 1 1 d . . . H21 H -0.1169 0.6084 0.1795 0.044 Uiso 1 1 calc R . . C22 C -0.0570(3) 0.69278(15) 0.12974(18) 0.0414(8) Uani 1 1 d . . . H22 H -0.1272 0.7189 0.1245 0.050 Uiso 1 1 calc R . . C23 C 0.0399(3) 0.72030(15) 0.10579(18) 0.0405(8) Uani 1 1 d . . . H23 H 0.0363 0.7656 0.0864 0.049 Uiso 1 1 calc R . . C24 C 0.1432(3) 0.68076(14) 0.11039(17) 0.0378(8) Uani 1 1 d . . . H24 H 0.2085 0.6998 0.0940 0.045 Uiso 1 1 calc R . . C25 C -0.0220(3) 0.49852(17) 0.23905(19) 0.0461(8) Uani 1 1 d . . . H25A H -0.0369 0.5349 0.2722 0.069 Uiso 1 1 calc R . . H25B H 0.0059 0.4571 0.2668 0.069 Uiso 1 1 calc R . . H25C H -0.0946 0.4880 0.2047 0.069 Uiso 1 1 calc R . . C26 C 0.3964(3) 0.61662(13) 0.11880(18) 0.0342(7) Uani 1 1 d . . . C27 C 0.3881(3) 0.64372(13) 0.04774(18) 0.0350(7) Uani 1 1 d . . . C28 C 0.4783(3) 0.68618(14) 0.03052(19) 0.0396(8) Uani 1 1 d . . . H28 H 0.4715 0.7052 -0.0165 0.048 Uiso 1 1 calc R . . C29 C 0.5786(3) 0.69953(15) 0.0849(2) 0.0470(9) Uani 1 1 d . . . H29 H 0.6390 0.7282 0.0740 0.056 Uiso 1 1 calc R . . C30 C 0.5903(3) 0.67114(15) 0.1545(2) 0.0431(8) Uani 1 1 d . . . H30 H 0.6592 0.6795 0.1898 0.052 Uiso 1 1 calc R . . C31 C 0.4990(3) 0.62987(13) 0.17208(19) 0.0369(8) Uani 1 1 d . . . H31 H 0.5063 0.6111 0.2193 0.044 Uiso 1 1 calc R . . C32 C 0.2633(3) 0.65853(17) -0.07282(19) 0.0515(9) Uani 1 1 d . . . H32A H 0.2606 0.7086 -0.0672 0.077 Uiso 1 1 calc R . . H32B H 0.1881 0.6423 -0.1007 0.077 Uiso 1 1 calc R . . H32C H 0.3262 0.6465 -0.0984 0.077 Uiso 1 1 calc R . . B1 B 0.7322(11) 0.6446(5) 0.3524(7) 0.043(3) Uani 0.584(9) 1 d PD A 1 F1 F 0.7955(10) 0.6122(4) 0.3050(5) 0.085(3) Uani 0.584(9) 1 d PD A 1 F2 F 0.7053(6) 0.7098(3) 0.3189(4) 0.0747(19) Uani 0.584(9) 1 d PD A 1 F3 F 0.7844(10) 0.6570(6) 0.4270(6) 0.090(3) Uani 0.584(9) 1 d PD A 1 F4 F 0.6183(5) 0.6161(3) 0.3512(3) 0.099(3) Uani 0.584(9) 1 d PD A 1 B2 B 0.7493(14) 0.6397(7) 0.3729(10) 0.059(7) Uani 0.416(9) 1 d PD A 2 F5 F 0.7182(12) 0.5766(4) 0.3923(5) 0.138(6) Uani 0.416(9) 1 d PD A 2 F6 F 0.6636(9) 0.6830(8) 0.3444(5) 0.105(5) Uani 0.416(9) 1 d PD A 2 F7 F 0.8080(17) 0.6199(10) 0.3236(10) 0.171(9) Uani 0.416(9) 1 d PD A 2 F8 F 0.8338(11) 0.6695(6) 0.4232(9) 0.071(3) Uani 0.416(9) 1 d PD 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 Cr1 0.0350(3) 0.0277(2) 0.0352(3) 0.0003(2) 0.0067(2) 0.0002(2) P1 0.0386(5) 0.0293(3) 0.0370(5) 0.0059(3) 0.0089(3) -0.0001(3) P2 0.0363(4) 0.0268(3) 0.0342(5) 0.0017(3) 0.0090(3) 0.0004(3) N1 0.0377(15) 0.0318(11) 0.0316(16) 0.0011(10) 0.0079(11) -0.0001(10) N2 0.0360(16) 0.0356(12) 0.061(2) -0.0089(13) 0.0040(14) 0.0026(11) O1 0.0506(15) 0.0471(12) 0.0351(15) -0.0001(10) 0.0028(11) -0.0020(10) O2 0.0605(16) 0.0368(11) 0.0506(16) -0.0031(10) 0.0031(12) 0.0051(10) O3 0.0352(14) 0.0479(12) 0.0614(17) 0.0001(11) 0.0082(11) -0.0014(11) O4 0.0376(14) 0.0481(12) 0.0477(16) 0.0031(10) 0.0135(11) 0.0044(10) O5 0.0499(15) 0.0425(12) 0.087(2) 0.0205(13) 0.0039(14) -0.0122(11) O6 0.0558(15) 0.0305(9) 0.0497(15) 0.0046(9) 0.0024(11) 0.0040(10) O7 0.0433(13) 0.0335(10) 0.0423(14) 0.0025(9) 0.0191(10) 0.0002(9) O8 0.0429(13) 0.0348(9) 0.0372(14) 0.0062(9) 0.0092(10) -0.0006(9) C1 0.052(2) 0.0368(15) 0.039(2) 0.0019(14) 0.0103(15) -0.0009(14) C2 0.048(2) 0.0286(13) 0.042(2) -0.0001(13) 0.0120(15) 0.0019(14) C3 0.044(2) 0.0284(13) 0.034(2) 0.0021(12) 0.0091(15) 0.0058(14) C4 0.0342(17) 0.0411(16) 0.033(2) 0.0026(13) 0.0040(13) 0.0039(13) C5 0.049(2) 0.0367(15) 0.056(3) 0.0180(15) 0.0208(17) 0.0063(15) C6 0.046(2) 0.0390(16) 0.088(3) 0.0242(19) 0.021(2) 0.0084(16) C7 0.057(3) 0.050(2) 0.129(5) 0.048(3) 0.043(3) 0.0107(19) C8 0.107(4) 0.069(3) 0.124(5) 0.060(3) 0.079(4) 0.032(3) C9 0.101(4) 0.065(2) 0.079(3) 0.036(2) 0.053(3) 0.021(3) C10 0.077(3) 0.0528(19) 0.051(3) 0.0246(18) 0.032(2) 0.0152(19) C11 0.062(3) 0.0443(19) 0.148(5) 0.024(2) -0.013(3) -0.0168(19) C12 0.0433(19) 0.0366(14) 0.0271(19) 0.0113(12) 0.0069(14) 0.0019(13) C13 0.047(2) 0.0410(15) 0.0277(19) 0.0120(13) 0.0071(14) 0.0032(14) C14 0.050(2) 0.0473(17) 0.040(2) 0.0136(15) 0.0090(16) 0.0116(16) C15 0.043(2) 0.066(2) 0.046(2) 0.0204(17) 0.0140(17) 0.0173(17) C16 0.041(2) 0.064(2) 0.044(2) 0.0170(17) 0.0047(16) -0.0025(17) C17 0.045(2) 0.0427(15) 0.036(2) 0.0123(14) 0.0083(15) 0.0024(14) C18 0.093(3) 0.0328(15) 0.052(3) 0.0075(15) -0.005(2) 0.0137(17) C19 0.0366(18) 0.0327(13) 0.031(2) -0.0055(12) 0.0088(13) 0.0016(12) C20 0.0442(19) 0.0310(13) 0.0291(19) -0.0055(12) 0.0094(14) 0.0001(13) C21 0.0349(17) 0.0384(14) 0.036(2) -0.0096(13) 0.0082(14) -0.0030(13) C22 0.042(2) 0.0410(15) 0.040(2) -0.0072(14) 0.0041(15) 0.0078(14) C23 0.046(2) 0.0310(13) 0.045(2) -0.0005(13) 0.0091(15) 0.0044(14) C24 0.0434(19) 0.0332(13) 0.037(2) -0.0005(13) 0.0093(14) 0.0005(13) C25 0.048(2) 0.0457(16) 0.050(2) 0.0071(15) 0.0210(16) 0.0005(15) C26 0.0391(18) 0.0218(11) 0.043(2) -0.0015(12) 0.0125(14) 0.0034(12) C27 0.0377(18) 0.0252(12) 0.044(2) 0.0027(12) 0.0116(15) 0.0037(12) C28 0.045(2) 0.0342(14) 0.044(2) 0.0063(13) 0.0193(16) -0.0021(13) C29 0.044(2) 0.0350(15) 0.066(3) 0.0012(16) 0.0206(18) -0.0061(14) C30 0.0399(19) 0.0349(14) 0.056(2) -0.0032(15) 0.0134(16) -0.0005(14) C31 0.0384(18) 0.0277(12) 0.046(2) 0.0006(12) 0.0122(15) 0.0027(13) C32 0.055(2) 0.0487(18) 0.051(2) 0.0197(16) 0.0109(17) 0.0063(16) B1 0.073(8) 0.043(5) 0.018(7) -0.013(4) 0.020(5) -0.011(5) F1 0.110(6) 0.105(4) 0.037(4) -0.024(3) 0.004(3) 0.066(4) F2 0.113(4) 0.062(3) 0.052(4) -0.015(2) 0.023(3) -0.016(3) F3 0.137(9) 0.086(4) 0.039(4) -0.002(3) 0.002(5) -0.027(5) F4 0.099(4) 0.088(4) 0.114(5) -0.006(3) 0.030(3) -0.051(3) B2 0.091(13) 0.060(8) 0.022(13) 0.019(8) 0.002(9) -0.022(8) F5 0.267(14) 0.056(4) 0.093(6) 0.000(4) 0.041(7) -0.063(6) F6 0.088(7) 0.169(12) 0.052(6) -0.019(6) -0.001(4) 0.074(8) F7 0.092(8) 0.323(19) 0.088(10) -0.145(10) -0.011(6) 0.051(8) F8 0.089(8) 0.061(5) 0.062(6) -0.011(4) 0.013(5) 0.008(5) _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 Cr1 N2 1.774(3) . yes Cr1 C4 1.840(3) . yes Cr1 C3 1.928(4) . yes Cr1 C2 1.944(4) . yes Cr1 P2 2.3816(9) . yes Cr1 P1 2.4295(11) . yes P1 N1 1.700(2) . yes P1 C5 1.808(4) . yes P1 C12 1.815(3) . yes P2 N1 1.693(2) . yes P2 C19 1.816(3) . yes P2 C26 1.824(3) . yes N1 C1 1.471(4) . yes N2 O1 1.164(3) . ? O2 C4 1.150(3) . ? O3 C2 1.137(4) . ? O4 C3 1.132(4) . ? O5 C6 1.349(5) . ? O5 C11 1.438(4) . ? O6 C13 1.366(4) . ? O6 C18 1.433(4) . ? O7 C20 1.364(3) . ? O7 C25 1.431(4) . ? O8 C27 1.365(3) . ? O8 C32 1.447(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C5 C10 1.406(5) . ? C5 C6 1.410(5) . ? C6 C7 1.399(6) . ? C7 C8 1.386(7) . ? C7 H7 0.9300 . ? C8 C9 1.385(7) . ? C8 H8 0.9300 . ? C9 C10 1.388(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C17 1.391(4) . ? C12 C13 1.410(4) . ? C13 C14 1.376(4) . ? C14 C15 1.387(5) . ? C14 H14 0.9300 . ? C15 C16 1.384(5) . ? C15 H15 0.9300 . ? C16 C17 1.392(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C24 1.399(4) . ? C19 C20 1.408(4) . ? C20 C21 1.394(4) . ? C21 C22 1.396(4) . ? C21 H21 0.9300 . ? C22 C23 1.372(5) . ? C22 H22 0.9300 . ? C23 C24 1.385(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C31 1.395(4) . ? C26 C27 1.395(4) . ? C27 C28 1.392(4) . ? C28 C29 1.388(4) . ? C28 H28 0.9300 . ? C29 C30 1.377(5) . ? C29 H29 0.9300 . ? C30 C31 1.392(4) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? B1 F1 1.384(10) . ? B1 F2 1.393(10) . ? B1 F4 1.403(11) . ? B1 F3 1.409(11) . ? B2 F7 1.287(14) . ? B2 F6 1.307(12) . ? B2 F5 1.321(12) . ? B2 F8 1.327(13) . ? 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 Cr1 C4 94.91(12) . . ? N2 Cr1 C3 88.75(13) . . ? C4 Cr1 C3 93.78(13) . . ? N2 Cr1 C2 90.23(13) . . ? C4 Cr1 C2 87.96(13) . . ? C3 Cr1 C2 178.06(11) . . ? N2 Cr1 P2 101.27(8) . . ? C4 Cr1 P2 163.80(10) . . ? C3 Cr1 P2 87.38(9) . . ? C2 Cr1 P2 91.19(9) . . ? N2 Cr1 P1 167.07(8) . . ? C4 Cr1 P1 96.46(10) . . ? C3 Cr1 P1 84.37(10) . . ? C2 Cr1 P1 96.31(10) . . ? P2 Cr1 P1 67.55(3) . . ? N1 P1 C5 108.58(15) . . yes N1 P1 C12 106.57(13) . . yes C5 P1 C12 102.46(14) . . yes N1 P1 Cr1 93.22(9) . . yes C5 P1 Cr1 128.47(12) . . ? C12 P1 Cr1 115.42(11) . . ? N1 P2 C19 107.75(14) . . yes N1 P2 C26 106.50(13) . . yes C19 P2 C26 105.80(13) . . yes N1 P2 Cr1 95.11(8) . . yes C19 P2 Cr1 123.93(9) . . ? C26 P2 Cr1 115.73(10) . . ? C1 N1 P2 123.82(18) . . ? C1 N1 P1 129.6(2) . . ? P2 N1 P1 104.07(13) . . ? O1 N2 Cr1 177.6(3) . . ? C6 O5 C11 117.4(3) . . ? C13 O6 C18 118.3(3) . . ? C20 O7 C25 117.8(2) . . ? C27 O8 C32 118.0(2) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O3 C2 Cr1 171.5(3) . . ? O4 C3 Cr1 177.8(3) . . ? O2 C4 Cr1 175.9(3) . . ? C10 C5 C6 118.7(4) . . ? C10 C5 P1 118.4(3) . . ? C6 C5 P1 122.8(3) . . ? O5 C6 C7 124.3(4) . . ? O5 C6 C5 116.5(3) . . ? C7 C6 C5 119.2(4) . . ? C8 C7 C6 120.1(4) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C9 C8 C7 121.9(4) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C10 118.1(5) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? C9 C10 C5 121.9(4) . . ? C9 C10 H10 119.1 . . ? C5 C10 H10 119.1 . . ? O5 C11 H11A 109.5 . . ? O5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 118.6(3) . . ? C17 C12 P1 124.2(2) . . ? C13 C12 P1 116.9(2) . . ? O6 C13 C14 125.1(3) . . ? O6 C13 C12 113.7(3) . . ? C14 C13 C12 121.3(3) . . ? C13 C14 C15 118.5(3) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C16 C15 C14 122.0(3) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 C17 118.9(3) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C12 C17 C16 120.7(3) . . ? C12 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? O6 C18 H18A 109.5 . . ? O6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 118.3(3) . . ? C24 C19 P2 120.8(3) . . ? C20 C19 P2 120.8(2) . . ? O7 C20 C21 123.1(3) . . ? O7 C20 C19 116.1(3) . . ? C21 C20 C19 120.7(3) . . ? C20 C21 C22 119.0(3) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C23 C22 C21 120.9(3) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 120.1(3) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 120.8(3) . . ? C23 C24 H24 119.6 . . ? C19 C24 H24 119.6 . . ? O7 C25 H25A 109.5 . . ? O7 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O7 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C31 C26 C27 119.3(3) . . ? C31 C26 P2 121.8(2) . . ? C27 C26 P2 118.6(2) . . ? O8 C27 C28 124.7(3) . . ? O8 C27 C26 114.5(3) . . ? C28 C27 C26 120.8(3) . . ? C29 C28 C27 118.8(3) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C30 C29 C28 121.2(3) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 119.9(3) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C26 119.9(3) . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? O8 C32 H32A 109.5 . . ? O8 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O8 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? F1 B1 F2 102.3(8) . . ? F1 B1 F4 114.4(9) . . ? F2 B1 F4 102.4(8) . . ? F1 B1 F3 121.4(10) . . ? F2 B1 F3 107.4(9) . . ? F4 B1 F3 107.0(9) . . ? F7 B2 F6 110.5(14) . . ? F7 B2 F5 97.5(16) . . ? F6 B2 F5 117.7(15) . . ? F7 B2 F8 102.3(14) . . ? F6 B2 F8 113.2(14) . . ? F5 B2 F8 113.3(12) . . ? 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 Cr1 P1 N1 29.8(4) . . . . ? C4 Cr1 P1 N1 -178.80(13) . . . . ? C3 Cr1 P1 N1 88.02(12) . . . . ? C2 Cr1 P1 N1 -90.15(12) . . . . ? P2 Cr1 P1 N1 -1.47(9) . . . . ? N2 Cr1 P1 C5 146.7(4) . . . . ? C4 Cr1 P1 C5 -61.91(17) . . . . ? C3 Cr1 P1 C5 -155.09(15) . . . . ? C2 Cr1 P1 C5 26.74(15) . . . . ? P2 Cr1 P1 C5 115.42(14) . . . . ? N2 Cr1 P1 C12 -80.2(4) . . . . ? C4 Cr1 P1 C12 71.14(14) . . . . ? C3 Cr1 P1 C12 -22.04(13) . . . . ? C2 Cr1 P1 C12 159.79(13) . . . . ? P2 Cr1 P1 C12 -111.53(11) . . . . ? N2 Cr1 P1 P2 31.3(4) . . . . ? C4 Cr1 P1 P2 -177.33(10) . . . . ? C3 Cr1 P1 P2 89.49(8) . . . . ? C2 Cr1 P1 P2 -88.68(8) . . . . ? N2 Cr1 P2 N1 -171.71(13) . . . . ? C4 Cr1 P2 N1 11.0(4) . . . . ? C3 Cr1 P2 N1 -83.51(13) . . . . ? C2 Cr1 P2 N1 97.81(13) . . . . ? P1 Cr1 P2 N1 1.48(9) . . . . ? N2 Cr1 P2 C19 72.88(16) . . . . ? C4 Cr1 P2 C19 -104.4(4) . . . . ? C3 Cr1 P2 C19 161.08(16) . . . . ? C2 Cr1 P2 C19 -17.60(16) . . . . ? P1 Cr1 P2 C19 -113.93(13) . . . . ? N2 Cr1 P2 C26 -60.63(14) . . . . ? C4 Cr1 P2 C26 122.1(4) . . . . ? C3 Cr1 P2 C26 27.57(14) . . . . ? C2 Cr1 P2 C26 -151.10(14) . . . . ? P1 Cr1 P2 C26 112.56(11) . . . . ? N2 Cr1 P2 P1 -173.19(9) . . . . ? C4 Cr1 P2 P1 9.5(4) . . . . ? C3 Cr1 P2 P1 -84.99(10) . . . . ? C2 Cr1 P2 P1 96.33(10) . . . . ? C5 P1 P2 N1 68.0(2) . . . . ? C12 P1 P2 N1 -76.51(19) . . . . ? Cr1 P1 P2 N1 -177.61(15) . . . . ? N1 P1 P2 C19 -71.75(18) . . . . ? C5 P1 P2 C19 -3.8(2) . . . . ? C12 P1 P2 C19 -148.26(16) . . . . ? Cr1 P1 P2 C19 110.64(12) . . . . ? N1 P1 P2 C26 75.63(19) . . . . ? C5 P1 P2 C26 143.6(2) . . . . ? C12 P1 P2 C26 -0.88(18) . . . . ? Cr1 P1 P2 C26 -101.98(13) . . . . ? N1 P1 P2 Cr1 177.61(15) . . . . ? C5 P1 P2 Cr1 -114.41(16) . . . . ? C12 P1 P2 Cr1 101.11(13) . . . . ? C19 P2 N1 C1 -37.5(3) . . . . ? C26 P2 N1 C1 75.7(3) . . . . ? Cr1 P2 N1 C1 -165.6(2) . . . . ? P1 P2 N1 C1 -163.6(3) . . . . ? C19 P2 N1 P1 126.09(14) . . . . ? C26 P2 N1 P1 -120.77(14) . . . . ? Cr1 P2 N1 P1 -2.01(12) . . . . ? C5 P1 N1 C1 31.6(3) . . . . ? C12 P1 N1 C1 -78.1(3) . . . . ? Cr1 P1 N1 C1 164.2(2) . . . . ? P2 P1 N1 C1 162.2(3) . . . . ? C5 P1 N1 P2 -130.58(16) . . . . ? C12 P1 N1 P2 119.70(15) . . . . ? Cr1 P1 N1 P2 1.97(12) . . . . ? N1 P1 C5 C10 -55.1(3) . . . . ? C12 P1 C5 C10 57.4(3) . . . . ? Cr1 P1 C5 C10 -165.2(2) . . . . ? P2 P1 C5 C10 -92.0(3) . . . . ? N1 P1 C5 C6 127.5(3) . . . . ? C12 P1 C5 C6 -120.0(3) . . . . ? Cr1 P1 C5 C6 17.4(3) . . . . yes P2 P1 C5 C6 90.6(3) . . . . ? C11 O5 C6 C7 -7.3(5) . . . . ? C11 O5 C6 C5 173.7(3) . . . . ? C10 C5 C6 O5 -176.8(3) . . . . ? P1 C5 C6 O5 0.5(4) . . . . ? C10 C5 C6 C7 4.1(5) . . . . ? P1 C5 C6 C7 -178.5(3) . . . . ? O5 C6 C7 C8 179.9(3) . . . . ? C5 C6 C7 C8 -1.1(5) . . . . ? C6 C7 C8 C9 -1.0(6) . . . . ? C7 C8 C9 C10 0.2(6) . . . . ? C8 C9 C10 C5 2.9(6) . . . . ? C6 C5 C10 C9 -5.1(5) . . . . ? P1 C5 C10 C9 177.4(3) . . . . ? N1 P1 C12 C17 1.8(3) . . . . ? C5 P1 C12 C17 -112.1(3) . . . . ? Cr1 P1 C12 C17 103.7(3) . . . . ? P2 P1 C12 C17 40.4(3) . . . . ? N1 P1 C12 C13 -172.4(2) . . . . ? C5 P1 C12 C13 73.6(3) . . . . ? Cr1 P1 C12 C13 -70.5(3) . . . . yes P2 P1 C12 C13 -133.9(2) . . . . ? C18 O6 C13 C14 -2.0(5) . . . . ? C18 O6 C13 C12 176.7(3) . . . . ? C17 C12 C13 O6 -178.6(3) . . . . ? P1 C12 C13 O6 -4.0(4) . . . . ? C17 C12 C13 C14 0.2(5) . . . . ? P1 C12 C13 C14 174.8(3) . . . . ? O6 C13 C14 C15 179.1(3) . . . . ? C12 C13 C14 C15 0.4(5) . . . . ? C13 C14 C15 C16 -0.3(5) . . . . ? C14 C15 C16 C17 -0.4(5) . . . . ? C13 C12 C17 C16 -0.9(5) . . . . ? P1 C12 C17 C16 -175.1(3) . . . . ? C15 C16 C17 C12 1.0(5) . . . . ? N1 P2 C19 C24 130.7(2) . . . . ? C26 P2 C19 C24 17.1(3) . . . . ? Cr1 P2 C19 C24 -120.1(2) . . . . ? P1 P2 C19 C24 168.65(19) . . . . ? N1 P2 C19 C20 -52.8(3) . . . . ? C26 P2 C19 C20 -166.4(2) . . . . ? Cr1 P2 C19 C20 56.3(3) . . . . yes P1 P2 C19 C20 -14.9(3) . . . . ? C25 O7 C20 C21 -9.4(4) . . . . ? C25 O7 C20 C19 169.9(3) . . . . ? C24 C19 C20 O7 -175.5(3) . . . . ? P2 C19 C20 O7 7.9(4) . . . . ? C24 C19 C20 C21 3.8(4) . . . . ? P2 C19 C20 C21 -172.8(2) . . . . ? O7 C20 C21 C22 178.1(3) . . . . ? C19 C20 C21 C22 -1.2(4) . . . . ? C20 C21 C22 C23 -2.2(4) . . . . ? C21 C22 C23 C24 2.8(5) . . . . ? C22 C23 C24 C19 0.0(5) . . . . ? C20 C19 C24 C23 -3.2(4) . . . . ? P2 C19 C24 C23 173.4(2) . . . . ? N1 P2 C26 C31 -2.9(3) . . . . ? C19 P2 C26 C31 111.6(2) . . . . ? Cr1 P2 C26 C31 -107.1(2) . . . . ? P1 P2 C26 C31 -41.4(3) . . . . ? N1 P2 C26 C27 170.7(2) . . . . ? C19 P2 C26 C27 -74.8(2) . . . . ? Cr1 P2 C26 C27 66.5(2) . . . . yes P1 P2 C26 C27 132.18(19) . . . . ? C32 O8 C27 C28 -6.9(4) . . . . ? C32 O8 C27 C26 172.4(3) . . . . ? C31 C26 C27 O8 177.8(2) . . . . ? P2 C26 C27 O8 4.1(3) . . . . ? C31 C26 C27 C28 -2.9(4) . . . . ? P2 C26 C27 C28 -176.6(2) . . . . ? O8 C27 C28 C29 -178.9(3) . . . . ? C26 C27 C28 C29 1.8(4) . . . . ? C27 C28 C29 C30 0.6(5) . . . . ? C28 C29 C30 C31 -1.9(5) . . . . ? C29 C30 C31 C26 0.8(4) . . . . ? C27 C26 C31 C30 1.5(4) . . . . ? P2 C26 C31 C30 175.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 70.07 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.445 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.059 data_lb125sad _database_code_depnum_ccdc_archive 'CCDC 626715' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H30 Cr O8 P2, C H2 Cl2' _chemical_formula_sum 'C34 H32 Cl2 Cr O8 P2' _chemical_formula_weight 753.44 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' 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' Cr Cr 0.3209 0.6236 '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' _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 11.807(9) _cell_length_b 17.767(11) _cell_length_c 17.847(9) _cell_angle_alpha 80.50(6) _cell_angle_beta 86.84(4) _cell_angle_gamma 74.80(6) _cell_volume 3563(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15763 _cell_measurement_theta_min 2.315 _cell_measurement_theta_max 27.650 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.726964 _exptl_absorpt_correction_T_max 0.910000 _exptl_absorpt_process_details 'SADABS V2.10 (Bruker AXS, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 37832 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 27.60 _reflns_number_total 16293 _reflns_number_gt 12015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.02 (Bruker, 1999)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+3.3509P] 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 16293 _refine_ls_number_parameters 855 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1224 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Cr1 Cr 0.88317(4) 0.61784(2) 0.22597(2) 0.02003(10) Uani 1 1 d . . . P1 P 0.82908(5) 0.71556(4) 0.30571(3) 0.01704(13) Uani 1 1 d . . . P2 P 0.96398(5) 0.72431(4) 0.17449(3) 0.01743(13) Uani 1 1 d . . . O1 O 1.10082(18) 0.54664(12) 0.32169(11) 0.0371(5) Uani 1 1 d . . . O2 O 0.6583(2) 0.69229(17) 0.13801(16) 0.0640(8) Uani 1 1 d . . . O3 O 0.7704(2) 0.49702(13) 0.31407(13) 0.0501(6) Uani 1 1 d . . . O4 O 0.9775(3) 0.51794(13) 0.10412(12) 0.0531(7) Uani 1 1 d . . . O5 O 0.86560(16) 0.82199(10) 0.40919(10) 0.0257(4) Uani 1 1 d . . . O6 O 0.61735(17) 0.67272(12) 0.35443(12) 0.0364(5) Uani 1 1 d . . . O7 O 1.09866(17) 0.84602(11) 0.15837(10) 0.0294(4) Uani 1 1 d . . . O8 O 0.95002(18) 0.69114(11) 0.02426(10) 0.0301(4) Uani 1 1 d . . . C1 C 0.9305(2) 0.77319(14) 0.25963(13) 0.0185(5) Uani 1 1 d . . . H1A H 0.8915 0.8302 0.2470 0.022 Uiso 1 1 calc R . . H1B H 1.0009 0.7656 0.2905 0.022 Uiso 1 1 calc R . . C2 C 1.0185(2) 0.57376(15) 0.28453(14) 0.0251(5) Uani 1 1 d . . . C3 C 0.7443(3) 0.66437(18) 0.17074(16) 0.0331(6) Uani 1 1 d . . . C4 C 0.8123(3) 0.54432(17) 0.27995(15) 0.0320(6) Uani 1 1 d . . . C5 C 0.9417(3) 0.55635(16) 0.15021(15) 0.0315(6) Uani 1 1 d . . . C6 C 0.8665(2) 0.69093(14) 0.40616(13) 0.0188(5) Uani 1 1 d . . . C7 C 0.8832(2) 0.74738(14) 0.44789(13) 0.0207(5) Uani 1 1 d . . . C8 C 0.9167(2) 0.72584(16) 0.52354(14) 0.0261(5) Uani 1 1 d . . . H8 H 0.9280 0.7644 0.5515 0.031 Uiso 1 1 calc R . . C9 C 0.9335(2) 0.64796(17) 0.55805(14) 0.0292(6) Uani 1 1 d . . . H9 H 0.9589 0.6331 0.6092 0.035 Uiso 1 1 calc R . . C10 C 0.9138(2) 0.59177(16) 0.51898(14) 0.0277(6) Uani 1 1 d . . . H10 H 0.9231 0.5389 0.5435 0.033 Uiso 1 1 calc R . . C11 C 0.8803(2) 0.61352(15) 0.44318(14) 0.0231(5) Uani 1 1 d . . . H11 H 0.8666 0.5750 0.4162 0.028 Uiso 1 1 calc R . . C12 C 0.8870(3) 0.88092(16) 0.44827(17) 0.0327(6) Uani 1 1 d . . . H12A H 0.8313 0.8885 0.4909 0.049 Uiso 1 1 calc R . . H12B H 0.8769 0.9308 0.4132 0.049 Uiso 1 1 calc R . . H12C H 0.9673 0.8638 0.4675 0.049 Uiso 1 1 calc R . . C13 C 0.6840(2) 0.78426(15) 0.30628(14) 0.0223(5) Uani 1 1 d . . . C14 C 0.5889(2) 0.75292(16) 0.33250(15) 0.0280(6) Uani 1 1 d . . . C15 C 0.4767(3) 0.80212(19) 0.3367(2) 0.0432(8) Uani 1 1 d . . . H15 H 0.4126 0.7807 0.3542 0.052 Uiso 1 1 calc R . . C16 C 0.4594(3) 0.8825(2) 0.3150(2) 0.0499(9) Uani 1 1 d . . . H16 H 0.3828 0.9163 0.3178 0.060 Uiso 1 1 calc R . . C17 C 0.5515(3) 0.91466(18) 0.2892(2) 0.0447(8) Uani 1 1 d . . . H17 H 0.5384 0.9701 0.2746 0.054 Uiso 1 1 calc R . . C18 C 0.6631(2) 0.86527(16) 0.28466(16) 0.0303(6) Uani 1 1 d . . . H18 H 0.7264 0.8873 0.2664 0.036 Uiso 1 1 calc R . . C19 C 0.5255(3) 0.6368(2) 0.3841(2) 0.0513(9) Uani 1 1 d . . . H19A H 0.4887 0.6605 0.4282 0.077 Uiso 1 1 calc R . . H19B H 0.5584 0.5800 0.3996 0.077 Uiso 1 1 calc R . . H19C H 0.4665 0.6454 0.3449 0.077 Uiso 1 1 calc R . . C20 C 1.1218(2) 0.71051(15) 0.16005(13) 0.0218(5) Uani 1 1 d . . . C21 C 1.1744(2) 0.77359(16) 0.15540(14) 0.0262(5) Uani 1 1 d . . . C22 C 1.2957(3) 0.7604(2) 0.15059(17) 0.0379(7) Uani 1 1 d . . . H22 H 1.3305 0.8032 0.1482 0.045 Uiso 1 1 calc R . . C23 C 1.3657(3) 0.6846(2) 0.14935(19) 0.0453(8) Uani 1 1 d . . . H23 H 1.4487 0.6756 0.1466 0.054 Uiso 1 1 calc R . . C24 C 1.3159(3) 0.6221(2) 0.15211(17) 0.0393(7) Uani 1 1 d . . . H24 H 1.3641 0.5704 0.1504 0.047 Uiso 1 1 calc R . . C25 C 1.1949(2) 0.63530(17) 0.15745(15) 0.0292(6) Uani 1 1 d . . . H25 H 1.1610 0.5921 0.1594 0.035 Uiso 1 1 calc R . . C26 C 1.1447(3) 0.91391(18) 0.14556(18) 0.0401(7) Uani 1 1 d . . . H26A H 1.1970 0.9115 0.1872 0.060 Uiso 1 1 calc R . . H26B H 1.0799 0.9618 0.1433 0.060 Uiso 1 1 calc R . . H26C H 1.1887 0.9151 0.0974 0.060 Uiso 1 1 calc R . . C27 C 0.8979(2) 0.79595(14) 0.09329(13) 0.0208(5) Uani 1 1 d . . . C28 C 0.8969(2) 0.76870(15) 0.02355(13) 0.0231(5) Uani 1 1 d . . . C29 C 0.8458(3) 0.82061(17) -0.04015(15) 0.0322(6) Uani 1 1 d . . . H29 H 0.8463 0.8022 -0.0872 0.039 Uiso 1 1 calc R . . C30 C 0.7948(3) 0.89870(18) -0.03471(17) 0.0400(7) Uani 1 1 d . . . H30 H 0.7596 0.9338 -0.0781 0.048 Uiso 1 1 calc R . . C31 C 0.7942(3) 0.92677(17) 0.03349(16) 0.0367(7) Uani 1 1 d . . . H31 H 0.7588 0.9807 0.0368 0.044 Uiso 1 1 calc R . . C32 C 0.8458(2) 0.87538(15) 0.09664(15) 0.0280(6) Uani 1 1 d . . . H32 H 0.8456 0.8947 0.1432 0.034 Uiso 1 1 calc R . . C33 C 0.9409(3) 0.65769(18) -0.04232(16) 0.0402(7) Uani 1 1 d . . . H33A H 0.8579 0.6651 -0.0534 0.060 Uiso 1 1 calc R . . H33B H 0.9801 0.6011 -0.0336 0.060 Uiso 1 1 calc R . . H33C H 0.9784 0.6840 -0.0855 0.060 Uiso 1 1 calc R . . Cr2 Cr 0.77588(3) 0.12010(2) 0.32669(2) 0.02018(10) Uani 1 1 d . . . P3 P 0.73173(5) 0.22696(4) 0.39613(3) 0.01778(13) Uani 1 1 d . . . P4 P 0.87373(6) 0.21535(4) 0.26763(3) 0.01911(13) Uani 1 1 d . . . O9 O 0.99629(17) 0.04818(12) 0.42005(11) 0.0337(4) Uani 1 1 d . . . O10 O 0.5605(2) 0.19076(17) 0.22895(17) 0.0684(8) Uani 1 1 d . . . O11 O 0.6341(2) 0.02267(13) 0.42536(14) 0.0472(6) Uani 1 1 d . . . O12 O 0.8596(2) -0.00261(13) 0.22494(13) 0.0497(6) Uani 1 1 d . . . O13 O 0.75989(17) 0.34672(11) 0.48633(10) 0.0276(4) Uani 1 1 d . . . O14 O 0.51604(16) 0.19638(11) 0.45383(12) 0.0340(4) Uani 1 1 d . . . O15 O 1.04428(17) 0.31699(11) 0.25616(11) 0.0291(4) Uani 1 1 d . . . O16 O 0.86304(18) 0.17137(11) 0.12139(10) 0.0320(4) Uani 1 1 d . . . C34 C 0.8424(2) 0.27432(14) 0.34601(13) 0.0200(5) Uani 1 1 d . . . H34A H 0.9122 0.2668 0.3774 0.024 Uiso 1 1 calc R . . H34B H 0.8093 0.3312 0.3277 0.024 Uiso 1 1 calc R . . C35 C 0.9118(2) 0.07529(14) 0.38555(14) 0.0237(5) Uani 1 1 d . . . C36 C 0.6422(3) 0.16581(18) 0.26548(17) 0.0361(7) Uani 1 1 d . . . C37 C 0.6882(2) 0.06012(16) 0.38814(16) 0.0301(6) Uani 1 1 d . . . C38 C 0.8267(3) 0.04555(16) 0.26308(15) 0.0304(6) Uani 1 1 d . . . C39 C 0.7680(2) 0.21216(15) 0.49687(13) 0.0204(5) Uani 1 1 d . . . C40 C 0.7795(2) 0.27509(15) 0.53168(14) 0.0222(5) Uani 1 1 d . . . C41 C 0.8110(2) 0.26164(17) 0.60786(14) 0.0274(6) Uani 1 1 d . . . H41 H 0.8183 0.3041 0.6317 0.033 Uiso 1 1 calc R . . C42 C 0.8314(2) 0.18598(17) 0.64856(14) 0.0291(6) Uani 1 1 d . . . H42 H 0.8535 0.1769 0.7003 0.035 Uiso 1 1 calc R . . C43 C 0.8203(2) 0.12368(17) 0.61516(14) 0.0274(6) Uani 1 1 d . . . H43 H 0.8347 0.0720 0.6435 0.033 Uiso 1 1 calc R . . C44 C 0.7876(2) 0.13744(15) 0.53936(14) 0.0239(5) Uani 1 1 d . . . H44 H 0.7785 0.0948 0.5164 0.029 Uiso 1 1 calc R . . C45 C 0.7666(3) 0.41353(17) 0.51902(18) 0.0378(7) Uani 1 1 d . . . H45A H 0.7099 0.4204 0.5612 0.057 Uiso 1 1 calc R . . H45B H 0.7485 0.4609 0.4804 0.057 Uiso 1 1 calc R . . H45C H 0.8460 0.4051 0.5380 0.057 Uiso 1 1 calc R . . C46 C 0.5896(2) 0.29951(15) 0.38952(14) 0.0218(5) Uani 1 1 d . . . C47 C 0.4915(2) 0.27319(15) 0.42016(15) 0.0262(5) Uani 1 1 d . . . C48 C 0.3803(2) 0.32523(18) 0.41628(18) 0.0365(7) Uani 1 1 d . . . H48 H 0.3144 0.3076 0.4374 0.044 Uiso 1 1 calc R . . C49 C 0.3659(3) 0.40252(18) 0.38176(19) 0.0397(7) Uani 1 1 d . . . H49 H 0.2897 0.4377 0.3788 0.048 Uiso 1 1 calc R . . C50 C 0.4610(3) 0.42920(17) 0.35141(19) 0.0387(7) Uani 1 1 d . . . H50 H 0.4506 0.4825 0.3277 0.046 Uiso 1 1 calc R . . C51 C 0.5717(2) 0.37750(16) 0.35586(16) 0.0305(6) Uani 1 1 d . . . H51 H 0.6371 0.3961 0.3353 0.037 Uiso 1 1 calc R . . C52 C 0.4198(3) 0.1641(2) 0.4820(2) 0.0445(8) Uani 1 1 d . . . H52A H 0.3777 0.1928 0.5219 0.067 Uiso 1 1 calc R . . H52B H 0.4497 0.1082 0.5031 0.067 Uiso 1 1 calc R . . H52C H 0.3661 0.1693 0.4404 0.067 Uiso 1 1 calc R . . C53 C 1.0337(2) 0.18704(14) 0.25438(13) 0.0216(5) Uani 1 1 d . . . C54 C 1.1036(2) 0.24104(15) 0.25108(14) 0.0244(5) Uani 1 1 d . . . C55 C 1.2251(2) 0.21641(17) 0.24306(16) 0.0316(6) Uani 1 1 d . . . H55 H 1.2714 0.2531 0.2412 0.038 Uiso 1 1 calc R . . C56 C 1.2783(2) 0.13773(17) 0.23778(17) 0.0342(6) Uani 1 1 d . . . H56 H 1.3613 0.1208 0.2327 0.041 Uiso 1 1 calc R . . C57 C 1.2117(2) 0.08397(17) 0.23983(16) 0.0313(6) Uani 1 1 d . . . H57 H 1.2485 0.0304 0.2356 0.038 Uiso 1 1 calc R . . C58 C 1.0903(2) 0.10882(16) 0.24810(14) 0.0262(5) Uani 1 1 d . . . H58 H 1.0450 0.0716 0.2495 0.031 Uiso 1 1 calc R . . C59 C 1.1093(3) 0.37569(17) 0.24126(17) 0.0356(7) Uani 1 1 d . . . H59A H 1.1723 0.3634 0.2783 0.053 Uiso 1 1 calc R . . H59B H 1.0567 0.4277 0.2454 0.053 Uiso 1 1 calc R . . H59C H 1.1433 0.3761 0.1899 0.053 Uiso 1 1 calc R . . C60 C 0.8218(2) 0.28364(15) 0.18080(13) 0.0236(5) Uani 1 1 d . . . C61 C 0.8201(2) 0.25137(16) 0.11411(14) 0.0267(5) Uani 1 1 d . . . C62 C 0.7800(3) 0.30031(19) 0.04670(16) 0.0379(7) Uani 1 1 d . . . H62 H 0.7788 0.2784 0.0018 0.045 Uiso 1 1 calc R . . C63 C 0.7420(3) 0.3808(2) 0.04525(17) 0.0482(9) Uani 1 1 d . . . H63 H 0.7143 0.4140 -0.0009 0.058 Uiso 1 1 calc R . . C64 C 0.7437(3) 0.41401(19) 0.11034(17) 0.0455(8) Uani 1 1 d . . . H64 H 0.7181 0.4696 0.1087 0.055 Uiso 1 1 calc R . . C65 C 0.7830(3) 0.36511(16) 0.17751(15) 0.0340(6) Uani 1 1 d . . . H65 H 0.7835 0.3876 0.2222 0.041 Uiso 1 1 calc R . . C66 C 0.8636(3) 0.13419(19) 0.05630(16) 0.0389(7) Uani 1 1 d . . . H66A H 0.7835 0.1464 0.0372 0.058 Uiso 1 1 calc R . . H66B H 0.8934 0.0769 0.0703 0.058 Uiso 1 1 calc R . . H66C H 0.9142 0.1537 0.0166 0.058 Uiso 1 1 calc R . . C67 C 0.4723(5) 0.1540(3) 0.9739(3) 0.110(2) Uani 1 1 d . . . H67A H 0.4865 0.2053 0.9507 0.132 Uiso 1 1 calc R . . H67B H 0.3864 0.1609 0.9777 0.132 Uiso 1 1 calc R . . Cl1 Cl 0.53298(13) 0.08299(10) 0.91305(9) 0.0985(4) Uani 1 1 d . . . Cl2 Cl 0.52777(16) 0.12945(11) 1.06156(11) 0.1171(6) Uani 1 1 d . . . C68 C 0.5404(5) 0.6582(3) 0.8992(3) 0.0932(17) Uani 1 1 d . . . H68A H 0.5488 0.7129 0.8869 0.112 Uiso 1 1 calc R . . H68B H 0.4555 0.6615 0.9055 0.112 Uiso 1 1 calc R . . Cl3 Cl 0.59224(16) 0.61049(10) 0.82320(9) 0.1120(6) Uani 1 1 d . . . Cl4 Cl 0.6056(2) 0.61715(15) 0.98267(11) 0.1720(10) 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 Cr1 0.0245(2) 0.0186(2) 0.01928(19) -0.00426(15) -0.00031(15) -0.00879(16) P1 0.0173(3) 0.0173(3) 0.0171(3) -0.0020(2) -0.0003(2) -0.0058(2) P2 0.0191(3) 0.0187(3) 0.0153(3) -0.0030(2) -0.0005(2) -0.0060(2) O1 0.0328(11) 0.0392(12) 0.0315(10) 0.0014(9) -0.0056(9) 0.0011(9) O2 0.0431(14) 0.081(2) 0.0704(18) 0.0012(15) -0.0299(13) -0.0213(14) O3 0.0759(17) 0.0392(13) 0.0477(13) -0.0097(10) 0.0178(12) -0.0383(13) O4 0.093(2) 0.0351(12) 0.0328(11) -0.0172(10) 0.0093(12) -0.0142(12) O5 0.0323(10) 0.0197(9) 0.0266(9) -0.0050(7) -0.0036(8) -0.0079(7) O6 0.0228(10) 0.0287(11) 0.0566(13) 0.0007(9) 0.0066(9) -0.0106(8) O7 0.0320(10) 0.0282(10) 0.0323(10) -0.0068(8) 0.0035(8) -0.0150(8) O8 0.0446(12) 0.0253(10) 0.0190(8) -0.0086(7) -0.0011(8) -0.0035(8) C1 0.0193(11) 0.0205(12) 0.0180(10) -0.0045(9) 0.0004(9) -0.0087(9) C2 0.0318(14) 0.0209(13) 0.0218(12) -0.0042(10) 0.0046(11) -0.0059(11) C3 0.0330(15) 0.0380(16) 0.0332(14) -0.0057(12) -0.0047(12) -0.0170(13) C4 0.0426(17) 0.0300(15) 0.0286(13) -0.0101(11) 0.0031(12) -0.0158(13) C5 0.0458(17) 0.0237(14) 0.0281(13) -0.0048(11) 0.0004(12) -0.0140(12) C6 0.0169(11) 0.0207(12) 0.0173(10) -0.0004(9) 0.0007(9) -0.0040(9) C7 0.0160(11) 0.0230(12) 0.0237(12) -0.0034(9) 0.0023(9) -0.0063(9) C8 0.0209(12) 0.0342(15) 0.0249(12) -0.0084(11) 0.0001(10) -0.0082(11) C9 0.0255(13) 0.0388(16) 0.0181(11) 0.0000(10) -0.0002(10) -0.0020(11) C10 0.0277(13) 0.0241(13) 0.0252(12) 0.0039(10) 0.0034(10) -0.0013(10) C11 0.0234(12) 0.0221(13) 0.0226(12) -0.0028(9) 0.0026(10) -0.0050(10) C12 0.0394(16) 0.0258(14) 0.0381(15) -0.0126(12) 0.0025(12) -0.0132(12) C13 0.0193(12) 0.0234(13) 0.0228(11) -0.0028(9) -0.0016(9) -0.0030(10) C14 0.0230(13) 0.0278(14) 0.0330(14) -0.0023(11) -0.0009(11) -0.0075(11) C15 0.0232(14) 0.0421(18) 0.060(2) 0.0009(15) 0.0030(14) -0.0079(13) C16 0.0262(15) 0.0411(19) 0.069(2) 0.0049(16) 0.0038(15) 0.0050(14) C17 0.0325(16) 0.0266(16) 0.063(2) 0.0085(14) 0.0026(15) 0.0034(13) C18 0.0245(13) 0.0245(14) 0.0390(15) 0.0010(11) 0.0052(11) -0.0061(11) C19 0.0354(17) 0.0398(19) 0.079(3) 0.0012(17) 0.0118(17) -0.0193(15) C20 0.0199(12) 0.0295(13) 0.0170(11) -0.0041(9) 0.0013(9) -0.0078(10) C21 0.0270(13) 0.0332(14) 0.0204(11) -0.0053(10) 0.0013(10) -0.0110(11) C22 0.0291(15) 0.0512(19) 0.0394(16) -0.0084(14) 0.0033(12) -0.0210(14) C23 0.0199(14) 0.065(2) 0.0495(19) -0.0085(16) 0.0027(13) -0.0093(14) C24 0.0276(15) 0.0431(18) 0.0401(16) -0.0026(13) 0.0019(12) 0.0008(13) C25 0.0277(14) 0.0329(15) 0.0250(12) -0.0024(11) 0.0008(11) -0.0057(11) C26 0.0507(19) 0.0348(17) 0.0426(17) -0.0071(13) 0.0082(14) -0.0258(15) C27 0.0223(12) 0.0217(12) 0.0187(11) -0.0008(9) -0.0014(9) -0.0075(10) C28 0.0250(13) 0.0248(13) 0.0202(11) -0.0036(10) 0.0015(10) -0.0079(10) C29 0.0416(16) 0.0345(15) 0.0212(12) -0.0039(11) -0.0056(11) -0.0101(13) C30 0.0508(19) 0.0348(16) 0.0284(14) 0.0050(12) -0.0115(13) -0.0046(14) C31 0.0508(19) 0.0247(14) 0.0305(14) -0.0018(11) -0.0077(13) -0.0024(13) C32 0.0367(15) 0.0235(13) 0.0238(12) -0.0035(10) -0.0012(11) -0.0076(11) C33 0.063(2) 0.0357(17) 0.0248(13) -0.0152(12) 0.0013(13) -0.0108(15) Cr2 0.0230(2) 0.0194(2) 0.02041(19) -0.00561(15) 0.00061(15) -0.00810(16) P3 0.0172(3) 0.0189(3) 0.0178(3) -0.0040(2) -0.0002(2) -0.0050(2) P4 0.0216(3) 0.0193(3) 0.0171(3) -0.0042(2) 0.0004(2) -0.0059(2) O9 0.0320(11) 0.0328(11) 0.0315(10) -0.0002(8) -0.0050(8) -0.0020(9) O10 0.0579(17) 0.0756(19) 0.0730(18) 0.0000(15) -0.0402(15) -0.0185(15) O11 0.0483(14) 0.0351(12) 0.0616(15) -0.0071(11) 0.0187(11) -0.0209(11) O12 0.0682(17) 0.0412(13) 0.0507(13) -0.0282(11) 0.0188(12) -0.0241(12) O13 0.0342(10) 0.0247(10) 0.0268(9) -0.0071(7) -0.0028(8) -0.0104(8) O14 0.0219(9) 0.0312(11) 0.0453(11) 0.0021(9) 0.0073(8) -0.0069(8) O15 0.0313(10) 0.0234(10) 0.0351(10) -0.0079(8) 0.0042(8) -0.0100(8) O16 0.0454(12) 0.0287(10) 0.0230(9) -0.0090(8) -0.0014(8) -0.0080(9) C34 0.0203(11) 0.0216(12) 0.0197(11) -0.0055(9) 0.0010(9) -0.0073(9) C35 0.0303(14) 0.0188(12) 0.0226(12) -0.0050(9) 0.0069(10) -0.0079(10) C36 0.0392(17) 0.0352(16) 0.0378(16) -0.0066(12) -0.0079(13) -0.0141(13) C37 0.0313(14) 0.0259(14) 0.0360(14) -0.0103(11) 0.0039(12) -0.0099(11) C38 0.0369(15) 0.0288(14) 0.0309(14) -0.0098(11) 0.0064(12) -0.0158(12) C39 0.0160(11) 0.0269(13) 0.0188(11) -0.0056(9) 0.0020(9) -0.0055(9) C40 0.0171(11) 0.0272(13) 0.0234(12) -0.0055(10) 0.0021(9) -0.0072(10) C41 0.0230(13) 0.0401(16) 0.0241(12) -0.0113(11) -0.0002(10) -0.0132(11) C42 0.0227(13) 0.0471(17) 0.0179(11) -0.0021(11) -0.0005(10) -0.0114(12) C43 0.0220(13) 0.0339(15) 0.0223(12) 0.0029(10) -0.0005(10) -0.0048(11) C44 0.0210(12) 0.0251(13) 0.0245(12) -0.0041(10) 0.0021(10) -0.0044(10) C45 0.0489(18) 0.0322(16) 0.0402(16) -0.0158(13) 0.0043(14) -0.0190(14) C46 0.0188(11) 0.0239(13) 0.0231(12) -0.0081(10) -0.0029(9) -0.0030(10) C47 0.0231(13) 0.0253(13) 0.0309(13) -0.0092(10) -0.0003(10) -0.0044(10) C48 0.0213(13) 0.0364(16) 0.0512(18) -0.0098(13) 0.0001(12) -0.0049(12) C49 0.0248(14) 0.0316(16) 0.059(2) -0.0115(14) -0.0063(13) 0.0026(12) C50 0.0355(16) 0.0226(14) 0.0543(19) -0.0016(13) -0.0068(14) -0.0025(12) C51 0.0277(14) 0.0246(14) 0.0394(15) -0.0056(11) -0.0032(12) -0.0062(11) C52 0.0325(16) 0.0420(18) 0.059(2) -0.0019(15) 0.0152(15) -0.0172(14) C53 0.0235(12) 0.0229(12) 0.0177(11) -0.0026(9) 0.0001(9) -0.0054(10) C54 0.0275(13) 0.0247(13) 0.0208(11) -0.0029(10) 0.0008(10) -0.0072(10) C55 0.0271(14) 0.0356(16) 0.0350(14) -0.0057(12) 0.0002(11) -0.0133(12) C56 0.0227(13) 0.0373(16) 0.0381(15) -0.0039(12) -0.0011(11) -0.0010(12) C57 0.0293(14) 0.0266(14) 0.0331(14) -0.0025(11) 0.0003(11) 0.0000(11) C58 0.0283(13) 0.0257(13) 0.0239(12) -0.0027(10) 0.0018(10) -0.0069(11) C59 0.0479(18) 0.0284(15) 0.0356(15) -0.0081(12) 0.0069(13) -0.0184(13) C60 0.0258(13) 0.0257(13) 0.0191(11) -0.0030(9) -0.0001(10) -0.0064(10) C61 0.0285(13) 0.0310(14) 0.0219(12) -0.0050(10) 0.0009(10) -0.0095(11) C62 0.0474(18) 0.0423(18) 0.0231(13) -0.0042(12) -0.0061(12) -0.0094(14) C63 0.068(2) 0.0424(19) 0.0255(14) 0.0066(13) -0.0119(15) -0.0037(17) C64 0.067(2) 0.0279(16) 0.0329(15) 0.0011(12) -0.0071(15) 0.0007(15) C65 0.0492(18) 0.0254(14) 0.0245(13) -0.0031(11) -0.0032(12) -0.0044(12) C66 0.0528(19) 0.0391(17) 0.0304(14) -0.0167(13) 0.0004(13) -0.0151(14) C67 0.076(3) 0.090(4) 0.124(5) 0.030(3) 0.043(3) 0.013(3) Cl1 0.0912(10) 0.1162(12) 0.1075(10) -0.0274(9) 0.0197(8) -0.0590(9) Cl2 0.1093(12) 0.1181(13) 0.1283(14) -0.0386(11) -0.0226(10) -0.0208(10) C68 0.082(4) 0.110(4) 0.076(3) -0.029(3) -0.005(3) 0.007(3) Cl3 0.1380(14) 0.1122(12) 0.1113(11) -0.0586(10) 0.0487(10) -0.0618(11) Cl4 0.211(2) 0.196(2) 0.0877(12) 0.0163(13) -0.0640(14) -0.0257(19) _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 Cr1 C4 1.845(3) . yes Cr1 C5 1.868(3) . yes Cr1 C2 1.875(3) . yes Cr1 C3 1.882(3) . yes Cr1 P1 2.3626(16) . yes Cr1 P2 2.3683(17) . yes P1 C13 1.825(3) . yes P1 C6 1.824(3) . yes P1 C1 1.848(3) . yes P2 C27 1.823(3) . yes P2 C20 1.824(3) . yes P2 C1 1.846(2) . yes O1 C2 1.156(3) . ? O2 C3 1.150(4) . ? O3 C4 1.156(4) . ? O4 C5 1.147(3) . ? O5 C7 1.359(3) . ? O5 C12 1.430(3) . ? O6 C14 1.370(3) . ? O6 C19 1.433(4) . ? O7 C21 1.368(3) . ? O7 C26 1.429(3) . ? O8 C28 1.355(3) . ? O8 C33 1.434(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C6 C11 1.396(4) . ? C6 C7 1.402(3) . ? C7 C8 1.391(3) . ? C8 C9 1.386(4) . ? C8 H8 0.9500 . ? C9 C10 1.381(4) . ? C9 H9 0.9500 . ? C10 C11 1.394(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.386(4) . ? C13 C14 1.405(4) . ? C14 C15 1.389(4) . ? C15 C16 1.380(5) . ? C15 H15 0.9500 . ? C16 C17 1.379(5) . ? C16 H16 0.9500 . ? C17 C18 1.385(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.394(4) . ? C20 C21 1.406(4) . ? C21 C22 1.389(4) . ? C22 C23 1.386(5) . ? C22 H22 0.9500 . ? C23 C24 1.379(5) . ? C23 H23 0.9500 . ? C24 C25 1.386(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C32 1.394(4) . ? C27 C28 1.410(3) . ? C28 C29 1.394(4) . ? C29 C30 1.377(4) . ? C29 H29 0.9500 . ? C30 C31 1.388(4) . ? C30 H30 0.9500 . ? C31 C32 1.385(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? Cr2 C38 1.846(3) . yes Cr2 C37 1.865(3) . yes Cr2 C35 1.885(3) . yes Cr2 C36 1.889(3) . yes Cr2 P3 2.3662(16) . yes Cr2 P4 2.3690(17) . yes P3 C46 1.824(3) . yes P3 C39 1.832(3) . yes P3 C34 1.847(3) . yes P4 C60 1.829(3) . yes P4 C53 1.835(3) . yes P4 C34 1.848(3) . yes O9 C35 1.150(3) . ? O10 C36 1.142(4) . ? O11 C37 1.150(4) . ? O12 C38 1.155(3) . ? O13 C40 1.362(3) . ? O13 C45 1.428(3) . ? O14 C47 1.360(3) . ? O14 C52 1.434(4) . ? O15 C54 1.363(3) . ? O15 C59 1.433(3) . ? O16 C61 1.365(3) . ? O16 C66 1.427(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C39 C44 1.385(4) . ? C39 C40 1.405(3) . ? C40 C41 1.395(4) . ? C41 C42 1.386(4) . ? C41 H41 0.9500 . ? C42 C43 1.379(4) . ? C42 H42 0.9500 . ? C43 C44 1.392(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C51 1.382(4) . ? C46 C47 1.411(4) . ? C47 C48 1.391(4) . ? C48 C49 1.380(4) . ? C48 H48 0.9500 . ? C49 C50 1.381(5) . ? C49 H49 0.9500 . ? C50 C51 1.384(4) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C58 1.395(4) . ? C53 C54 1.413(4) . ? C54 C55 1.393(4) . ? C55 C56 1.391(4) . ? C55 H55 0.9500 . ? C56 C57 1.383(4) . ? C56 H56 0.9500 . ? C57 C58 1.392(4) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C65 1.391(4) . ? C60 C61 1.407(3) . ? C61 C62 1.389(4) . ? C62 C63 1.378(5) . ? C62 H62 0.9500 . ? C63 C64 1.391(4) . ? C63 H63 0.9500 . ? C64 C65 1.383(4) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 Cl2 1.674(7) . ? C67 Cl1 1.783(6) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 Cl4 1.678(5) . ? C68 Cl3 1.718(5) . ? C68 H68A 0.9900 . ? C68 H68B 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 C4 Cr1 C5 93.89(13) . . ? C4 Cr1 C2 89.93(14) . . ? C5 Cr1 C2 92.39(13) . . ? C4 Cr1 C3 89.58(14) . . ? C5 Cr1 C3 90.11(14) . . ? C2 Cr1 C3 177.48(12) . . ? C4 Cr1 P1 98.64(10) . . ? C5 Cr1 P1 167.47(9) . . ? C2 Cr1 P1 87.80(9) . . ? C3 Cr1 P1 89.83(10) . . ? C4 Cr1 P2 170.11(9) . . ? C5 Cr1 P2 95.95(10) . . ? C2 Cr1 P2 88.74(10) . . ? C3 Cr1 P2 91.32(11) . . ? P1 Cr1 P2 71.52(5) . . yes C13 P1 C6 102.89(12) . . yes C13 P1 C1 106.74(13) . . yes C6 P1 C1 106.42(11) . . yes C13 P1 Cr1 123.81(9) . . ? C6 P1 Cr1 120.18(9) . . ? C1 P1 Cr1 94.52(9) . . yes C27 P2 C20 104.86(12) . . yes C27 P2 C1 107.64(12) . . yes C20 P2 C1 104.25(11) . . yes C27 P2 Cr1 121.33(9) . . ? C20 P2 Cr1 121.58(10) . . ? C1 P2 Cr1 94.37(9) . . yes C7 O5 C12 117.6(2) . . ? C14 O6 C19 118.0(2) . . ? C21 O7 C26 118.4(2) . . ? C28 O8 C33 117.8(2) . . ? P2 C1 P1 96.92(12) . . yes P2 C1 H1A 112.4 . . ? P1 C1 H1A 112.4 . . ? P2 C1 H1B 112.4 . . ? P1 C1 H1B 112.4 . . ? H1A C1 H1B 109.9 . . ? O1 C2 Cr1 178.9(2) . . ? O2 C3 Cr1 178.8(3) . . ? O3 C4 Cr1 178.4(3) . . ? O4 C5 Cr1 179.3(3) . . ? C11 C6 C7 118.3(2) . . ? C11 C6 P1 119.60(19) . . ? C7 C6 P1 122.05(18) . . ? O5 C7 C8 123.9(2) . . ? O5 C7 C6 115.5(2) . . ? C8 C7 C6 120.6(2) . . ? C7 C8 C9 119.8(2) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 120.8(2) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 119.3(2) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C10 C11 C6 121.2(2) . . ? C10 C11 H11 119.4 . . ? C6 C11 H11 119.4 . . ? O5 C12 H12A 109.5 . . ? O5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 118.4(2) . . ? C18 C13 P1 123.9(2) . . ? C14 C13 P1 117.6(2) . . ? O6 C14 C15 124.5(3) . . ? O6 C14 C13 114.9(2) . . ? C15 C14 C13 120.6(3) . . ? C16 C15 C14 119.3(3) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 121.2(3) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 119.3(3) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 121.2(3) . . ? C13 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? O6 C19 H19A 109.5 . . ? O6 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O6 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 117.9(2) . . ? C25 C20 P2 120.2(2) . . ? C21 C20 P2 121.7(2) . . ? O7 C21 C22 123.9(3) . . ? O7 C21 C20 115.5(2) . . ? C22 C21 C20 120.6(3) . . ? C23 C22 C21 119.9(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.5(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.5(3) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C24 C25 C20 121.5(3) . . ? C24 C25 H25 119.2 . . ? C20 C25 H25 119.2 . . ? O7 C26 H26A 109.5 . . ? O7 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O7 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 118.2(2) . . ? C32 C27 P2 123.91(19) . . ? C28 C27 P2 117.85(19) . . ? O8 C28 C29 124.6(2) . . ? O8 C28 C27 115.0(2) . . ? C29 C28 C27 120.3(2) . . ? C30 C29 C28 119.9(3) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 120.8(3) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C32 C31 C30 119.4(3) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C31 C32 C27 121.4(2) . . ? C31 C32 H32 119.3 . . ? C27 C32 H32 119.3 . . ? O8 C33 H33A 109.5 . . ? O8 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O8 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C38 Cr2 C37 93.36(13) . . ? C38 Cr2 C35 90.06(13) . . ? C37 Cr2 C35 93.03(13) . . ? C38 Cr2 C36 89.30(14) . . ? C37 Cr2 C36 88.42(14) . . ? C35 Cr2 C36 178.45(13) . . ? C38 Cr2 P3 170.49(9) . . ? C37 Cr2 P3 96.12(9) . . ? C35 Cr2 P3 88.62(9) . . ? C36 Cr2 P3 91.77(11) . . ? C38 Cr2 P4 98.96(10) . . ? C37 Cr2 P4 167.67(8) . . ? C35 Cr2 P4 86.45(10) . . ? C36 Cr2 P4 92.24(11) . . ? P3 Cr2 P4 71.55(5) . . yes C46 P3 C39 103.69(12) . . yes C46 P3 C34 108.37(13) . . yes C39 P3 C34 104.88(12) . . yes C46 P3 Cr2 121.89(9) . . ? C39 P3 Cr2 121.15(10) . . ? C34 P3 Cr2 94.59(9) . . yes C60 P4 C53 103.65(12) . . yes C60 P4 C34 106.49(12) . . yes C53 P4 C34 107.09(12) . . yes C60 P4 Cr2 123.13(10) . . ? C53 P4 Cr2 119.82(10) . . ? C34 P4 Cr2 94.49(9) . . yes C40 O13 C45 118.5(2) . . ? C47 O14 C52 118.1(2) . . ? C54 O15 C59 117.3(2) . . ? C61 O16 C66 118.4(2) . . ? P3 C34 P4 97.04(12) . . yes P3 C34 H34A 112.4 . . ? P4 C34 H34A 112.4 . . ? P3 C34 H34B 112.4 . . ? P4 C34 H34B 112.4 . . ? H34A C34 H34B 109.9 . . ? O9 C35 Cr2 178.5(2) . . ? O10 C36 Cr2 177.4(3) . . ? O11 C37 Cr2 179.2(2) . . ? O12 C38 Cr2 178.2(3) . . ? C44 C39 C40 119.0(2) . . ? C44 C39 P3 119.81(19) . . ? C40 C39 P3 121.13(19) . . ? O13 C40 C41 124.2(2) . . ? O13 C40 C39 115.8(2) . . ? C41 C40 C39 119.9(2) . . ? C42 C41 C40 119.6(2) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C43 C42 C41 121.1(2) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C42 C43 C44 119.2(3) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C39 C44 C43 121.1(2) . . ? C39 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? O13 C45 H45A 109.5 . . ? O13 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O13 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C51 C46 C47 118.2(2) . . ? C51 C46 P3 124.6(2) . . ? C47 C46 P3 117.1(2) . . ? O14 C47 C48 124.9(3) . . ? O14 C47 C46 115.0(2) . . ? C48 C47 C46 120.1(3) . . ? C49 C48 C47 120.0(3) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 120.7(3) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C49 C50 C51 119.3(3) . . ? C49 C50 H50 120.4 . . ? C51 C50 H50 120.4 . . ? C46 C51 C50 121.7(3) . . ? C46 C51 H51 119.1 . . ? C50 C51 H51 119.1 . . ? O14 C52 H52A 109.5 . . ? O14 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O14 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C58 C53 C54 117.8(2) . . ? C58 C53 P4 119.4(2) . . ? C54 C53 P4 122.86(19) . . ? O15 C54 C55 123.4(2) . . ? O15 C54 C53 115.7(2) . . ? C55 C54 C53 120.9(2) . . ? C56 C55 C54 119.6(3) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? C57 C56 C55 120.7(3) . . ? C57 C56 H56 119.7 . . ? C55 C56 H56 119.7 . . ? C56 C57 C58 119.5(3) . . ? C56 C57 H57 120.2 . . ? C58 C57 H57 120.2 . . ? C57 C58 C53 121.6(3) . . ? C57 C58 H58 119.2 . . ? C53 C58 H58 119.2 . . ? O15 C59 H59A 109.5 . . ? O15 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? O15 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C65 C60 C61 118.6(2) . . ? C65 C60 P4 123.6(2) . . ? C61 C60 P4 117.7(2) . . ? O16 C61 C62 124.6(2) . . ? O16 C61 C60 115.1(2) . . ? C62 C61 C60 120.3(3) . . ? C63 C62 C61 119.8(3) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 121.0(3) . . ? C62 C63 H63 119.5 . . ? C64 C63 H63 119.5 . . ? C65 C64 C63 119.1(3) . . ? C65 C64 H64 120.4 . . ? C63 C64 H64 120.4 . . ? C64 C65 C60 121.2(3) . . ? C64 C65 H65 119.4 . . ? C60 C65 H65 119.4 . . ? O16 C66 H66A 109.5 . . ? O16 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? O16 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? Cl2 C67 Cl1 113.8(3) . . ? Cl2 C67 H67A 108.8 . . ? Cl1 C67 H67A 108.8 . . ? Cl2 C67 H67B 108.8 . . ? Cl1 C67 H67B 108.8 . . ? H67A C67 H67B 107.7 . . ? Cl4 C68 Cl3 116.2(3) . . ? Cl4 C68 H68A 108.2 . . ? Cl3 C68 H68A 108.2 . . ? Cl4 C68 H68B 108.2 . . ? Cl3 C68 H68B 108.2 . . ? H68A C68 H68B 107.4 . . ? 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 C4 Cr1 P1 C13 -78.54(15) . . . . ? C5 Cr1 P1 C13 100.8(5) . . . . ? C2 Cr1 P1 C13 -168.14(13) . . . . ? C3 Cr1 P1 C13 11.01(14) . . . . ? P2 Cr1 P1 C13 102.46(12) . . . . ? C4 Cr1 P1 C6 55.89(14) . . . . ? C5 Cr1 P1 C6 -124.8(4) . . . . ? C2 Cr1 P1 C6 -33.71(13) . . . . ? C3 Cr1 P1 C6 145.44(13) . . . . ? P2 Cr1 P1 C6 -123.11(10) . . . . ? C4 Cr1 P1 C1 167.85(12) . . . . ? C5 Cr1 P1 C1 -12.9(4) . . . . ? C2 Cr1 P1 C1 78.25(12) . . . . ? C3 Cr1 P1 C1 -102.60(13) . . . . ? P2 Cr1 P1 C1 -11.15(8) . . . . ? C5 Cr1 P2 C27 77.07(14) . . . . ? C2 Cr1 P2 C27 169.34(12) . . . . ? C3 Cr1 P2 C27 -13.18(13) . . . . ? P1 Cr1 P2 C27 -102.56(11) . . . . ? C5 Cr1 P2 C20 -59.54(14) . . . . ? C2 Cr1 P2 C20 32.73(12) . . . . ? C3 Cr1 P2 C20 -149.79(13) . . . . ? P1 Cr1 P2 C20 120.83(10) . . . . ? C5 Cr1 P2 C1 -169.21(12) . . . . ? C2 Cr1 P2 C1 -76.95(12) . . . . ? C3 Cr1 P2 C1 100.54(13) . . . . ? P1 Cr1 P2 C1 11.16(8) . . . . ? C27 P2 C1 P1 111.18(13) . . . . ? C20 P2 C1 P1 -137.82(12) . . . . ? Cr1 P2 C1 P1 -13.68(9) . . . . ? C13 P1 C1 P2 -113.63(12) . . . . ? C6 P1 C1 P2 137.01(11) . . . . ? Cr1 P1 C1 P2 13.71(9) . . . . ? C13 P1 C6 C11 115.6(2) . . . . ? C1 P1 C6 C11 -132.4(2) . . . . ? Cr1 P1 C6 C11 -26.9(2) . . . . ? C13 P1 C6 C7 -65.1(2) . . . . ? C1 P1 C6 C7 47.0(2) . . . . ? Cr1 P1 C6 C7 152.44(17) . . . . yes C12 O5 C7 C8 2.2(4) . . . . ? C12 O5 C7 C6 -177.1(2) . . . . ? C11 C6 C7 O5 -178.4(2) . . . . ? P1 C6 C7 O5 2.2(3) . . . . ? C11 C6 C7 C8 2.2(4) . . . . ? P1 C6 C7 C8 -177.15(19) . . . . ? O5 C7 C8 C9 -179.4(2) . . . . ? C6 C7 C8 C9 -0.1(4) . . . . ? C7 C8 C9 C10 -2.1(4) . . . . ? C8 C9 C10 C11 2.1(4) . . . . ? C9 C10 C11 C6 0.1(4) . . . . ? C7 C6 C11 C10 -2.2(4) . . . . ? P1 C6 C11 C10 177.16(19) . . . . ? C6 P1 C13 C18 104.2(2) . . . . ? C1 P1 C13 C18 -7.6(3) . . . . ? Cr1 P1 C13 C18 -115.1(2) . . . . ? C6 P1 C13 C14 -73.8(2) . . . . ? C1 P1 C13 C14 174.39(19) . . . . ? Cr1 P1 C13 C14 66.9(2) . . . . yes C19 O6 C14 C15 -0.4(4) . . . . ? C19 O6 C14 C13 178.0(3) . . . . ? C18 C13 C14 O6 -178.5(2) . . . . ? P1 C13 C14 O6 -0.4(3) . . . . ? C18 C13 C14 C15 -0.1(4) . . . . ? P1 C13 C14 C15 178.0(2) . . . . ? O6 C14 C15 C16 178.1(3) . . . . ? C13 C14 C15 C16 -0.2(5) . . . . ? C14 C15 C16 C17 0.1(6) . . . . ? C15 C16 C17 C18 0.3(6) . . . . ? C14 C13 C18 C17 0.5(4) . . . . ? P1 C13 C18 C17 -177.5(2) . . . . ? C16 C17 C18 C13 -0.6(5) . . . . ? C27 P2 C20 C25 -123.6(2) . . . . ? C1 P2 C20 C25 123.4(2) . . . . ? Cr1 P2 C20 C25 19.0(2) . . . . ? C27 P2 C20 C21 59.9(2) . . . . ? C1 P2 C20 C21 -53.1(2) . . . . ? Cr1 P2 C20 C21 -157.45(17) . . . . yes C26 O7 C21 C22 8.8(4) . . . . ? C26 O7 C21 C20 -173.2(2) . . . . ? C25 C20 C21 O7 -179.9(2) . . . . ? P2 C20 C21 O7 -3.3(3) . . . . ? C25 C20 C21 C22 -1.8(4) . . . . ? P2 C20 C21 C22 174.7(2) . . . . ? O7 C21 C22 C23 178.7(3) . . . . ? C20 C21 C22 C23 0.9(4) . . . . ? C21 C22 C23 C24 0.6(5) . . . . ? C22 C23 C24 C25 -1.1(5) . . . . ? C23 C24 C25 C20 0.1(4) . . . . ? C21 C20 C25 C24 1.4(4) . . . . ? P2 C20 C25 C24 -175.2(2) . . . . ? C20 P2 C27 C32 -103.1(2) . . . . ? C1 P2 C27 C32 7.4(3) . . . . ? Cr1 P2 C27 C32 114.1(2) . . . . ? C20 P2 C27 C28 78.7(2) . . . . ? C1 P2 C27 C28 -170.74(19) . . . . ? Cr1 P2 C27 C28 -64.1(2) . . . . yes C33 O8 C28 C29 -8.0(4) . . . . ? C33 O8 C28 C27 173.3(2) . . . . ? C32 C27 C28 O8 179.4(2) . . . . ? P2 C27 C28 O8 -2.3(3) . . . . ? C32 C27 C28 C29 0.7(4) . . . . ? P2 C27 C28 C29 179.0(2) . . . . ? O8 C28 C29 C30 -179.5(3) . . . . ? C27 C28 C29 C30 -0.9(4) . . . . ? C28 C29 C30 C31 0.5(5) . . . . ? C29 C30 C31 C32 0.0(5) . . . . ? C30 C31 C32 C27 -0.2(5) . . . . ? C28 C27 C32 C31 -0.1(4) . . . . ? P2 C27 C32 C31 -178.3(2) . . . . ? C37 Cr2 P3 C46 -75.81(15) . . . . ? C35 Cr2 P3 C46 -168.71(13) . . . . ? C36 Cr2 P3 C46 12.79(14) . . . . ? P4 Cr2 P3 C46 104.57(12) . . . . ? C37 Cr2 P3 C39 58.75(14) . . . . ? C35 Cr2 P3 C39 -34.15(12) . . . . ? C36 Cr2 P3 C39 147.36(14) . . . . ? P4 Cr2 P3 C39 -120.87(11) . . . . ? C37 Cr2 P3 C34 169.21(12) . . . . ? C35 Cr2 P3 C34 76.31(12) . . . . ? C36 Cr2 P3 C34 -102.19(14) . . . . ? P4 Cr2 P3 C34 -10.41(8) . . . . ? C38 Cr2 P4 C60 78.14(15) . . . . ? C37 Cr2 P4 C60 -104.4(4) . . . . ? C35 Cr2 P4 C60 167.65(12) . . . . ? C36 Cr2 P4 C60 -11.50(14) . . . . ? P3 Cr2 P4 C60 -102.62(11) . . . . ? C38 Cr2 P4 C53 -56.20(14) . . . . ? C37 Cr2 P4 C53 121.3(4) . . . . ? C35 Cr2 P4 C53 33.31(12) . . . . ? C36 Cr2 P4 C53 -145.84(13) . . . . ? P3 Cr2 P4 C53 123.04(10) . . . . ? C38 Cr2 P4 C34 -168.83(12) . . . . ? C37 Cr2 P4 C34 8.6(4) . . . . ? C35 Cr2 P4 C34 -79.32(12) . . . . ? C36 Cr2 P4 C34 101.53(13) . . . . ? P3 Cr2 P4 C34 10.41(8) . . . . ? C46 P3 C34 P4 -113.01(12) . . . . ? C39 P3 C34 P4 136.73(12) . . . . ? Cr2 P3 C34 P4 12.79(10) . . . . ? C60 P4 C34 P3 113.73(13) . . . . ? C53 P4 C34 P3 -135.87(12) . . . . ? Cr2 P4 C34 P3 -12.78(10) . . . . ? C46 P3 C39 C44 121.5(2) . . . . ? C34 P3 C39 C44 -124.9(2) . . . . ? Cr2 P3 C39 C44 -20.0(2) . . . . ? C46 P3 C39 C40 -60.2(2) . . . . ? C34 P3 C39 C40 53.4(2) . . . . ? Cr2 P3 C39 C40 158.35(16) . . . . yes C45 O13 C40 C41 -2.9(4) . . . . ? C45 O13 C40 C39 178.1(2) . . . . ? C44 C39 C40 O13 179.5(2) . . . . ? P3 C39 C40 O13 1.2(3) . . . . ? C44 C39 C40 C41 0.4(4) . . . . ? P3 C39 C40 C41 -177.92(19) . . . . ? O13 C40 C41 C42 -178.6(2) . . . . ? C39 C40 C41 C42 0.4(4) . . . . ? C40 C41 C42 C43 -0.6(4) . . . . ? C41 C42 C43 C44 -0.2(4) . . . . ? C40 C39 C44 C43 -1.2(4) . . . . ? P3 C39 C44 C43 177.19(19) . . . . ? C42 C43 C44 C39 1.0(4) . . . . ? C39 P3 C46 C51 107.9(2) . . . . ? C34 P3 C46 C51 -3.2(2) . . . . ? Cr2 P3 C46 C51 -111.0(2) . . . . ? C39 P3 C46 C47 -73.1(2) . . . . ? C34 P3 C46 C47 175.89(18) . . . . ? Cr2 P3 C46 C47 68.1(2) . . . . yes C52 O14 C47 C48 5.5(4) . . . . ? C52 O14 C47 C46 -176.2(2) . . . . ? C51 C46 C47 O14 -178.6(2) . . . . ? P3 C46 C47 O14 2.3(3) . . . . ? C51 C46 C47 C48 -0.2(4) . . . . ? P3 C46 C47 C48 -179.3(2) . . . . ? O14 C47 C48 C49 178.9(3) . . . . ? C46 C47 C48 C49 0.6(4) . . . . ? C47 C48 C49 C50 -0.6(5) . . . . ? C48 C49 C50 C51 0.0(5) . . . . ? C47 C46 C51 C50 -0.3(4) . . . . ? P3 C46 C51 C50 178.7(2) . . . . ? C49 C50 C51 C46 0.4(5) . . . . ? C60 P4 C53 C58 -114.9(2) . . . . ? C34 P4 C53 C58 132.7(2) . . . . ? Cr2 P4 C53 C58 27.0(2) . . . . ? C60 P4 C53 C54 65.8(2) . . . . ? C34 P4 C53 C54 -46.5(2) . . . . ? Cr2 P4 C53 C54 -152.20(17) . . . . yes C59 O15 C54 C55 9.4(4) . . . . ? C59 O15 C54 C53 -170.5(2) . . . . ? C58 C53 C54 O15 178.9(2) . . . . ? P4 C53 C54 O15 -1.9(3) . . . . ? C58 C53 C54 C55 -1.0(4) . . . . ? P4 C53 C54 C55 178.2(2) . . . . ? O15 C54 C55 C56 -179.6(2) . . . . ? C53 C54 C55 C56 0.4(4) . . . . ? C54 C55 C56 C57 0.5(4) . . . . ? C55 C56 C57 C58 -0.7(4) . . . . ? C56 C57 C58 C53 0.0(4) . . . . ? C54 C53 C58 C57 0.8(4) . . . . ? P4 C53 C58 C57 -178.4(2) . . . . ? C53 P4 C60 C65 -104.6(3) . . . . ? C34 P4 C60 C65 8.2(3) . . . . ? Cr2 P4 C60 C65 115.1(2) . . . . ? C53 P4 C60 C61 76.1(2) . . . . ? C34 P4 C60 C61 -171.1(2) . . . . ? Cr2 P4 C60 C61 -64.2(2) . . . . yes C66 O16 C61 C62 -2.3(4) . . . . ? C66 O16 C61 C60 179.6(2) . . . . ? C65 C60 C61 O16 178.0(2) . . . . ? P4 C60 C61 O16 -2.7(3) . . . . ? C65 C60 C61 C62 -0.2(4) . . . . ? P4 C60 C61 C62 179.1(2) . . . . ? O16 C61 C62 C63 -177.9(3) . . . . ? C60 C61 C62 C63 0.1(5) . . . . ? C61 C62 C63 C64 0.3(5) . . . . ? C62 C63 C64 C65 -0.7(6) . . . . ? C63 C64 C65 C60 0.6(5) . . . . ? C61 C60 C65 C64 -0.2(5) . . . . ? P4 C60 C65 C64 -179.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.015 _refine_diff_density_min -1.151 _refine_diff_density_rms 0.075