# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name M.E.O'Reilly 'T.J.Del Castillo' K.A.Abboud A.S.Veige _publ_contact_author_name 'Adam S. Veige' _publ_contact_author_email veige@chem.ufl.edu data_orei20 _database_code_depnum_ccdc_archive 'CCDC 829370' #TrackingRef '- orei20.cif' _audit_update_record ; 2010-05-24 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H60 Cr O3 P' _chemical_formula_weight 900.04 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.0808(10) _cell_length_b 16.9424(15) _cell_length_c 25.884(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.572(2) _cell_angle_gamma 90.00 _cell_volume 4760.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 315 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1908 _exptl_absorpt_coefficient_mu 0.320 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9227 _exptl_absorpt_correction_T_max 0.9805 _exptl_absorpt_process_details 'based on measured indexed crystal faces, Bruker SHELXTL v6.12 (Bruker 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 58088 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10940 _reflns_number_gt 7354 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT (Bruker, 2008)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2008)' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The asymmetric unit consists of the Cr complex and two toluene solvent molecules. ; _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^)+(0.0385P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10940 _refine_ls_number_parameters 593 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _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 -0.02176(2) 0.678067(16) 0.199136(10) 0.01154(7) Uani 1 1 d . . . P1 P 0.25815(4) 0.66896(3) 0.281788(17) 0.01238(10) Uani 1 1 d . . . O1 O 0.08348(10) 0.69983(7) 0.15321(4) 0.0133(3) Uani 1 1 d . . . O2 O -0.04929(10) 0.62415(7) 0.25818(4) 0.0127(3) Uani 1 1 d . . . O4 O -0.12546(10) 0.74245(7) 0.18691(4) 0.0156(3) Uani 1 1 d . . . C1 C 0.05076(15) 0.70106(10) 0.09995(7) 0.0141(4) Uani 1 1 d . . . C2 C 0.08671(15) 0.76578(10) 0.07169(7) 0.0155(4) Uani 1 1 d . . . C3 C 0.05464(16) 0.76205(11) 0.01691(7) 0.0193(4) Uani 1 1 d . . . H3A H 0.0787 0.8040 -0.0032 0.023 Uiso 1 1 calc R . . C4 C -0.01122(17) 0.69932(11) -0.00943(7) 0.0220(4) Uani 1 1 d . . . H4A H -0.0316 0.6989 -0.0469 0.026 Uiso 1 1 calc R . . C5 C -0.04696(16) 0.63763(11) 0.01886(7) 0.0201(4) Uani 1 1 d . . . H5A H -0.0936 0.5953 0.0008 0.024 Uiso 1 1 calc R . . C6 C -0.01522(15) 0.63679(10) 0.07394(7) 0.0153(4) Uani 1 1 d . . . C7 C -0.05420(15) 0.57055(10) 0.10414(7) 0.0158(4) Uani 1 1 d . . . C8 C -0.06873(16) 0.49586(11) 0.08008(7) 0.0202(4) Uani 1 1 d . . . H8A H -0.0463 0.4884 0.0469 0.024 Uiso 1 1 calc R . . C9 C -0.11504(17) 0.43320(11) 0.10396(7) 0.0228(4) Uani 1 1 d . . . H9A H -0.1194 0.3823 0.0883 0.027 Uiso 1 1 calc R . . C10 C -0.15514(16) 0.44451(11) 0.15057(7) 0.0207(4) Uani 1 1 d . . . H10A H -0.1911 0.4018 0.1659 0.025 Uiso 1 1 calc R . . C11 C -0.14340(15) 0.51848(10) 0.17559(7) 0.0160(4) Uani 1 1 d . . . C12 C -0.08331(15) 0.58079(10) 0.15449(6) 0.0136(4) Uani 1 1 d . . . C13 C -0.19997(15) 0.52836(10) 0.22239(7) 0.0148(4) Uani 1 1 d . . . C14 C -0.30588(16) 0.48552(10) 0.22657(7) 0.0182(4) Uani 1 1 d . . . H14A H -0.3413 0.4502 0.1992 0.022 Uiso 1 1 calc R . . C15 C -0.35891(16) 0.49412(10) 0.26986(7) 0.0190(4) Uani 1 1 d . . . H15A H -0.4307 0.4649 0.2724 0.023 Uiso 1 1 calc R . . C16 C -0.30729(16) 0.54563(10) 0.30981(7) 0.0165(4) Uani 1 1 d . . . H16A H -0.3443 0.5503 0.3397 0.020 Uiso 1 1 calc R . . C17 C -0.20338(15) 0.5908(1) 0.30786(7) 0.0146(4) Uani 1 1 d . . . C18 C -0.15061(15) 0.58167(10) 0.26223(6) 0.0130(4) Uani 1 1 d . . . C19 C 0.15514(16) 0.83734(10) 0.09971(7) 0.0171(4) Uani 1 1 d . . . C20 C 0.07685(16) 0.87769(11) 0.13510(7) 0.0194(4) Uani 1 1 d . . . H20A H 0.0547 0.8389 0.1597 0.029 Uiso 1 1 calc R . . H20B H 0.0017 0.8992 0.1131 0.029 Uiso 1 1 calc R . . H20C H 0.1243 0.9206 0.1550 0.029 Uiso 1 1 calc R . . C21 C 0.27985(16) 0.81084(11) 0.13247(7) 0.0216(4) Uani 1 1 d . . . H21A H 0.3297 0.7875 0.1091 0.032 Uiso 1 1 calc R . . H21B H 0.2663 0.7715 0.1585 0.032 Uiso 1 1 calc R . . H21C H 0.3231 0.8565 0.1507 0.032 Uiso 1 1 calc R . . C22 C 0.18226(18) 0.90019(11) 0.06050(7) 0.0266(5) Uani 1 1 d . . . H22A H 0.2340 0.8771 0.0378 0.040 Uiso 1 1 calc R . . H22B H 0.2254 0.9449 0.0800 0.040 Uiso 1 1 calc R . . H22C H 0.1046 0.9185 0.0387 0.040 Uiso 1 1 calc R . . C23 C -0.14692(16) 0.64615(10) 0.35292(7) 0.0158(4) Uani 1 1 d . . . C24 C -0.22187(18) 0.64866(12) 0.39681(7) 0.0239(4) Uani 1 1 d . . . H24A H -0.2269 0.5955 0.4111 0.036 Uiso 1 1 calc R . . H24B H -0.3051 0.6681 0.3823 0.036 Uiso 1 1 calc R . . H24C H -0.1814 0.6840 0.4250 0.036 Uiso 1 1 calc R . . C25 C -0.01661(16) 0.61678(11) 0.37748(7) 0.0203(4) Uani 1 1 d . . . H25A H -0.0217 0.5638 0.3921 0.030 Uiso 1 1 calc R . . H25B H 0.0214 0.6529 0.4057 0.030 Uiso 1 1 calc R . . H25C H 0.0335 0.6149 0.3503 0.030 Uiso 1 1 calc R . . C26 C -0.14297(16) 0.73131(10) 0.33244(7) 0.0185(4) Uani 1 1 d . . . H26A H -0.2272 0.7506 0.3202 0.028 Uiso 1 1 calc R . . H26B H -0.0990 0.7322 0.3032 0.028 Uiso 1 1 calc R . . H26C H -0.1002 0.7653 0.3610 0.028 Uiso 1 1 calc R . . C27 C 0.12806(15) 0.72714(11) 0.25569(7) 0.0131(4) Uani 1 1 d . . . H27B H 0.0885(17) 0.7422(11) 0.2829(7) 0.022(5) Uiso 1 1 d . . . H27A H 0.1549(16) 0.7720(11) 0.2404(7) 0.022(5) Uiso 1 1 d . . . C28 C 0.22757(15) 0.56504(10) 0.27224(7) 0.0137(4) Uani 1 1 d . . . C29 C 0.19606(15) 0.53553(11) 0.22083(7) 0.0162(4) Uani 1 1 d . . . H29A H 0.1971 0.5694 0.1917 0.019 Uiso 1 1 calc R . . C30 C 0.16351(16) 0.45723(11) 0.21240(7) 0.0192(4) Uani 1 1 d . . . H30A H 0.1422 0.4373 0.1775 0.023 Uiso 1 1 calc R . . C31 C 0.16182(16) 0.40750(11) 0.25503(7) 0.0208(4) Uani 1 1 d . . . H31A H 0.1388 0.3537 0.2491 0.025 Uiso 1 1 calc R . . C32 C 0.19354(16) 0.43618(11) 0.30607(7) 0.0193(4) Uani 1 1 d . . . H32A H 0.1929 0.4020 0.3351 0.023 Uiso 1 1 calc R . . C33 C 0.22625(15) 0.5147(1) 0.31487(7) 0.0171(4) Uani 1 1 d . . . H33A H 0.2478 0.5343 0.3499 0.021 Uiso 1 1 calc R . . C34 C 0.31162(15) 0.68516(10) 0.35194(6) 0.0131(4) Uani 1 1 d . . . C35 C 0.24543(16) 0.73106(10) 0.38103(7) 0.0158(4) Uani 1 1 d . . . H35A H 0.1701 0.7548 0.3642 0.019 Uiso 1 1 calc R . . C36 C 0.28948(16) 0.74222(11) 0.43480(7) 0.0183(4) Uani 1 1 d . . . H36A H 0.2441 0.7736 0.4547 0.022 Uiso 1 1 calc R . . C37 C 0.39882(16) 0.70784(11) 0.45930(7) 0.0188(4) Uani 1 1 d . . . H37A H 0.4283 0.7154 0.4960 0.023 Uiso 1 1 calc R . . C38 C 0.46596(16) 0.66223(11) 0.43053(7) 0.0194(4) Uani 1 1 d . . . H38A H 0.5414 0.6387 0.4475 0.023 Uiso 1 1 calc R . . C39 C 0.42260(16) 0.65115(10) 0.37713(7) 0.0175(4) Uani 1 1 d . . . H39A H 0.4687 0.6201 0.3574 0.021 Uiso 1 1 calc R . . C40 C 0.38801(15) 0.69619(10) 0.25313(7) 0.0149(4) Uani 1 1 d . . . C41 C 0.43710(16) 0.77163(11) 0.26495(7) 0.0190(4) Uani 1 1 d . . . H41A H 0.4013 0.8060 0.2867 0.023 Uiso 1 1 calc R . . C42 C 0.53760(16) 0.79637(12) 0.24500(7) 0.0235(4) Uani 1 1 d . . . H42A H 0.5712 0.8475 0.2533 0.028 Uiso 1 1 calc R . . C43 C 0.58942(16) 0.74632(12) 0.21274(7) 0.0233(4) Uani 1 1 d . . . H43A H 0.6576 0.7636 0.1985 0.028 Uiso 1 1 calc R . . C44 C 0.54205(17) 0.67213(12) 0.20147(7) 0.0229(4) Uani 1 1 d . . . H44A H 0.5782 0.6381 0.1796 0.028 Uiso 1 1 calc R . . C45 C 0.44184(16) 0.64601(11) 0.22156(7) 0.0185(4) Uani 1 1 d . . . H45A H 0.4102 0.5943 0.2138 0.022 Uiso 1 1 calc R . . C46 C 0.3300(2) 0.61256(14) 0.0563(1) 0.0517(7) Uani 1 1 d . . . H46A H 0.2420 0.6135 0.0404 0.078 Uiso 1 1 calc R . . H46B H 0.3773 0.6327 0.0309 0.078 Uiso 1 1 calc R . . H46C H 0.3453 0.6458 0.0879 0.078 Uiso 1 1 calc R . . C47 C 0.36889(19) 0.52945(12) 0.07111(8) 0.0285(5) Uani 1 1 d . . . C48 C 0.2891(2) 0.47767(13) 0.08775(8) 0.0344(5) Uani 1 1 d . . . H48A H 0.2087 0.4948 0.0900 0.041 Uiso 1 1 calc R . . C49 C 0.3246(3) 0.40071(15) 0.10124(10) 0.0498(7) Uani 1 1 d . . . H49A H 0.2684 0.3658 0.1128 0.060 Uiso 1 1 calc R . . C50 C 0.4400(3) 0.37441(14) 0.09804(9) 0.0471(7) Uani 1 1 d . . . H50A H 0.4639 0.3215 0.1071 0.057 Uiso 1 1 calc R . . C51 C 0.5205(2) 0.42574(15) 0.08157(9) 0.0440(6) Uani 1 1 d . . . H51A H 0.6008 0.4083 0.0793 0.053 Uiso 1 1 calc R . . C52 C 0.4857(2) 0.50216(14) 0.06833(9) 0.0404(6) Uani 1 1 d . . . H52A H 0.5425 0.5370 0.0571 0.048 Uiso 1 1 calc R . . C53 C 0.66168(19) 0.72172(12) 0.07202(8) 0.0335(5) Uani 1 1 d . . . H53A H 0.7380 0.7037 0.0950 0.050 Uiso 1 1 calc R . . H53B H 0.6509 0.6945 0.0380 0.050 Uiso 1 1 calc R . . H53C H 0.5916 0.7099 0.0886 0.050 Uiso 1 1 calc R . . C54 C 0.66863(16) 0.80959(12) 0.06348(7) 0.0218(4) Uani 1 1 d . . . C55 C 0.58130(17) 0.86084(12) 0.07668(7) 0.0254(5) Uani 1 1 d . . . H55A H 0.5185 0.8406 0.0932 0.031 Uiso 1 1 calc R . . C56 C 0.58461(18) 0.94090(13) 0.06612(8) 0.0304(5) Uani 1 1 d . . . H56A H 0.5232 0.9748 0.0746 0.037 Uiso 1 1 calc R . . C57 C 0.67667(19) 0.97157(13) 0.04330(7) 0.0310(5) Uani 1 1 d . . . H57A H 0.6790 1.0264 0.0360 0.037 Uiso 1 1 calc R . . C58 C 0.76512(19) 0.92169(13) 0.03130(7) 0.0309(5) Uani 1 1 d . . . H58A H 0.8298 0.9425 0.0162 0.037 Uiso 1 1 calc R . . C59 C 0.76096(17) 0.84156(12) 0.04092(7) 0.0265(5) Uani 1 1 d . . . H59A H 0.8222 0.8080 0.0319 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.01208(13) 0.01201(15) 0.01063(14) -0.00049(12) 0.00251(10) -0.00006(11) P1 0.0129(2) 0.0129(2) 0.0113(2) 0.00005(18) 0.00218(17) 0.00026(18) O1 0.0147(6) 0.0158(7) 0.0097(6) 0.0005(5) 0.0032(5) -0.0011(5) O2 0.0138(6) 0.0141(6) 0.0107(6) 0.0003(5) 0.0038(5) -0.0035(5) O4 0.0148(6) 0.0154(7) 0.0162(6) -0.0017(5) 0.0022(5) 0.0013(5) C1 0.0134(8) 0.0182(10) 0.0115(9) 0.0002(7) 0.0041(7) 0.0041(7) C2 0.0151(9) 0.0179(10) 0.0145(9) 0.0011(7) 0.0055(7) 0.0038(7) C3 0.0212(9) 0.0219(11) 0.0165(10) 0.0035(8) 0.0082(8) 0.0061(8) C4 0.026(1) 0.0306(12) 0.0098(9) -0.0003(8) 0.0048(8) 0.0079(8) C5 0.0217(10) 0.0230(11) 0.0157(10) -0.0057(8) 0.0039(8) 0.0021(8) C6 0.0150(9) 0.0177(10) 0.0140(9) -0.0019(7) 0.0048(7) 0.0021(7) C7 0.0133(8) 0.0176(10) 0.0164(9) -0.0037(7) 0.0025(7) 0.0005(7) C8 0.0212(9) 0.0223(11) 0.0182(10) -0.0071(8) 0.0064(8) -0.0014(8) C9 0.025(1) 0.0156(10) 0.0293(11) -0.0091(8) 0.0095(9) -0.0040(8) C10 0.0227(10) 0.0164(10) 0.0247(11) -0.0035(8) 0.0090(8) -0.0056(8) C11 0.0138(8) 0.0164(10) 0.0172(9) -0.0022(7) 0.0017(7) 0.0005(7) C12 0.0124(8) 0.0139(9) 0.0139(9) -0.0026(7) 0.0012(7) 0.0007(7) C13 0.0169(9) 0.0126(9) 0.0158(9) 0.0023(7) 0.0050(7) 0.0006(7) C14 0.0213(9) 0.0126(10) 0.0203(10) -0.0017(8) 0.0028(8) -0.0035(7) C15 0.0177(9) 0.018(1) 0.0222(10) 0.0025(8) 0.0061(8) -0.0045(7) C16 0.0173(9) 0.0165(10) 0.0171(9) 0.0028(8) 0.0068(7) 0.0019(7) C17 0.0155(9) 0.0144(10) 0.0138(9) 0.0020(7) 0.0025(7) 0.0025(7) C18 0.0141(8) 0.0107(9) 0.0142(9) 0.0038(7) 0.0032(7) 0.0014(7) C19 0.0197(9) 0.0158(10) 0.0169(9) 0.0036(7) 0.0059(7) -0.0007(7) C20 0.0226(10) 0.0162(10) 0.020(1) -0.0002(8) 0.0055(8) -0.0003(8) C21 0.0188(9) 0.0222(11) 0.0239(10) 0.0021(8) 0.0048(8) -0.0024(8) C22 0.0340(11) 0.0224(11) 0.0251(11) 0.0051(9) 0.0104(9) -0.0040(9) C23 0.0180(9) 0.019(1) 0.0112(9) 0.0001(7) 0.0048(7) -0.0006(7) C24 0.0281(11) 0.0294(12) 0.0164(10) -0.0035(8) 0.0096(8) -0.0062(8) C25 0.0213(10) 0.0231(11) 0.0154(10) 0.0006(8) 0.0010(8) -0.0006(8) C26 0.0230(9) 0.0173(10) 0.016(1) -0.0020(8) 0.0061(8) 0.0009(8) C27 0.0142(9) 0.0125(10) 0.0130(9) -0.0011(7) 0.0035(7) 0.0000(7) C28 0.0122(8) 0.0127(9) 0.0161(9) 0.0014(7) 0.0027(7) 0.0009(7) C29 0.0183(9) 0.0169(10) 0.0132(9) 0.0022(7) 0.0024(7) 0.0035(7) C30 0.0233(10) 0.017(1) 0.0165(10) -0.0038(8) 0.0022(8) 0.0020(8) C31 0.0238(10) 0.0128(10) 0.0256(11) -0.0019(8) 0.0047(8) -0.0011(8) C32 0.0225(10) 0.0158(10) 0.0201(10) 0.0042(8) 0.0058(8) 0.0002(8) C33 0.0166(9) 0.0198(10) 0.0149(9) -0.0003(8) 0.0032(7) 0.0015(7) C34 0.0139(8) 0.0121(9) 0.0136(9) 0.0010(7) 0.0032(7) -0.0015(7) C35 0.0150(9) 0.0163(10) 0.0157(9) 0.0027(7) 0.0021(7) 0.0010(7) C36 0.0224(9) 0.0183(10) 0.0146(9) -0.0017(8) 0.0050(7) 0.0007(8) C37 0.0218(10) 0.0211(10) 0.0121(9) 0.0003(7) -0.0003(7) -0.0024(8) C38 0.0154(9) 0.0219(11) 0.0194(10) 0.0036(8) -0.0004(7) 0.0012(8) C39 0.0170(9) 0.0176(10) 0.0181(10) -0.0005(7) 0.0040(7) 0.0014(7) C40 0.0128(8) 0.0174(10) 0.0143(9) 0.0034(7) 0.0021(7) 0.0018(7) C41 0.0165(9) 0.0197(10) 0.0214(10) 0.0002(8) 0.0052(7) 0.0012(8) C42 0.0170(9) 0.0222(11) 0.0300(11) 0.0057(9) 0.0020(8) -0.0012(8) C43 0.0141(9) 0.0312(12) 0.0259(11) 0.0114(9) 0.0071(8) 0.0028(8) C44 0.0222(10) 0.0273(11) 0.0215(10) 0.0060(9) 0.0096(8) 0.0075(9) C45 0.0190(9) 0.018(1) 0.0192(10) 0.0021(8) 0.0056(8) 0.0032(7) C46 0.0583(17) 0.0355(15) 0.0622(17) 0.0098(13) 0.0141(14) 0.0110(12) C47 0.0302(11) 0.0254(12) 0.0292(12) -0.0004(9) 0.0045(9) 0.0019(9) C48 0.0318(12) 0.0383(14) 0.0366(13) -0.0021(10) 0.0152(10) 0.0006(10) C49 0.0684(18) 0.0369(15) 0.0522(16) 0.0033(12) 0.0313(14) -0.0101(13) C50 0.0748(19) 0.0294(14) 0.0358(14) 0.0037(11) 0.0077(13) 0.0157(13) C51 0.0353(13) 0.0465(16) 0.0479(15) -0.0051(12) 0.0031(11) 0.0130(12) C52 0.0299(12) 0.0383(14) 0.0548(16) -0.0011(12) 0.0129(11) 0.0002(10) C53 0.0346(12) 0.0353(13) 0.0277(12) 0.0016(10) -0.0008(9) 0.0003(10) C54 0.0186(9) 0.0315(12) 0.0129(9) -0.0020(8) -0.0028(7) -0.0007(8) C55 0.0178(10) 0.0397(13) 0.019(1) -0.0080(9) 0.0041(8) -0.0058(9) C56 0.0264(11) 0.0367(14) 0.0267(12) -0.0117(10) 0.0017(9) 0.0044(9) C57 0.0392(13) 0.0296(12) 0.0210(11) -0.0018(9) -0.0017(9) -0.0038(10) C58 0.0285(11) 0.0467(15) 0.0182(11) -0.0006(10) 0.0063(9) -0.0095(10) C59 0.0201(10) 0.0411(14) 0.0179(10) -0.0051(9) 0.0027(8) 0.0030(9) _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 O4 1.5699(11) . ? Cr1 O2 1.8576(11) . ? Cr1 O1 1.8615(11) . ? Cr1 C12 2.0495(17) . ? Cr1 C27 2.1483(17) . ? P1 C27 1.7650(17) . ? P1 C28 1.8007(18) . ? P1 C40 1.8060(17) . ? P1 C34 1.8144(17) . ? O1 C1 1.3535(19) . ? O2 C18 1.3551(19) . ? C1 C6 1.406(2) . ? C1 C2 1.419(2) . ? C2 C3 1.392(2) . ? C2 C19 1.533(2) . ? C3 C4 1.388(3) . ? C3 H3A 0.9500 . ? C4 C5 1.379(3) . ? C4 H4A 0.9500 . ? C5 C6 1.398(2) . ? C5 H5A 0.9500 . ? C6 C7 1.481(2) . ? C7 C8 1.405(2) . ? C7 C12 1.415(2) . ? C8 C9 1.378(2) . ? C8 H8A 0.9500 . ? C9 C10 1.380(2) . ? C9 H9A 0.9500 . ? C10 C11 1.405(2) . ? C10 H10A 0.9500 . ? C11 C12 1.415(2) . ? C11 C13 1.481(2) . ? C13 C18 1.397(2) . ? C13 C14 1.402(2) . ? C14 C15 1.374(2) . ? C14 H14A 0.9500 . ? C15 C16 1.386(2) . ? C15 H15A 0.9500 . ? C16 C17 1.392(2) . ? C16 H16A 0.9500 . ? C17 C18 1.428(2) . ? C17 C23 1.529(2) . ? C19 C21 1.536(2) . ? C19 C22 1.541(2) . ? C19 C20 1.542(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.536(2) . ? C23 C25 1.539(2) . ? C23 C26 1.541(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27B 0.938(18) . ? C27 H27A 0.933(19) . ? C28 C33 1.397(2) . ? C28 C29 1.399(2) . ? C29 C30 1.381(2) . ? C29 H29A 0.9500 . ? C30 C31 1.391(2) . ? C30 H30A 0.9500 . ? C31 C32 1.385(2) . ? C31 H31A 0.9500 . ? C32 C33 1.385(2) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 C35 1.390(2) . ? C34 C39 1.396(2) . ? C35 C36 1.392(2) . ? C35 H35A 0.9500 . ? C36 C37 1.379(2) . ? C36 H36A 0.9500 . ? C37 C38 1.388(2) . ? C37 H37A 0.9500 . ? C38 C39 1.382(2) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 C45 1.394(2) . ? C40 C41 1.399(2) . ? C41 C42 1.383(2) . ? C41 H41A 0.9500 . ? C42 C43 1.392(3) . ? C42 H42A 0.9500 . ? C43 C44 1.371(3) . ? C43 H43A 0.9500 . ? C44 C45 1.390(2) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 C47 1.500(3) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.375(3) . ? C47 C52 1.390(3) . ? C48 C49 1.386(3) . ? C48 H48A 0.9500 . ? C49 C50 1.373(3) . ? C49 H49A 0.9500 . ? C50 C51 1.373(3) . ? C50 H50A 0.9500 . ? C51 C52 1.375(3) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? C53 C54 1.509(3) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C59 1.386(3) . ? C54 C55 1.393(3) . ? C55 C56 1.386(3) . ? C55 H55A 0.9500 . ? C56 C57 1.379(3) . ? C56 H56A 0.9500 . ? C57 C58 1.376(3) . ? C57 H57A 0.9500 . ? C58 C59 1.383(3) . ? C58 H58A 0.9500 . ? C59 H59A 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 O4 Cr1 O2 105.86(6) . . ? O4 Cr1 O1 105.10(6) . . ? O2 Cr1 O1 148.23(5) . . ? O4 Cr1 C12 107.32(6) . . ? O2 Cr1 C12 88.71(6) . . ? O1 Cr1 C12 88.82(6) . . ? O4 Cr1 C27 107.62(6) . . ? O2 Cr1 C27 82.05(6) . . ? O1 Cr1 C27 82.01(6) . . ? C12 Cr1 C27 145.05(7) . . ? C27 P1 C28 112.13(8) . . ? C27 P1 C40 110.91(8) . . ? C28 P1 C40 109.69(8) . . ? C27 P1 C34 112.10(8) . . ? C28 P1 C34 107.45(8) . . ? C40 P1 C34 104.20(8) . . ? C1 O1 Cr1 125.4(1) . . ? C18 O2 Cr1 126.87(10) . . ? O1 C1 C6 118.91(15) . . ? O1 C1 C2 119.43(15) . . ? C6 C1 C2 121.63(15) . . ? C3 C2 C1 116.69(16) . . ? C3 C2 C19 121.25(16) . . ? C1 C2 C19 122.05(15) . . ? C4 C3 C2 122.45(17) . . ? C4 C3 H3A 118.8 . . ? C2 C3 H3A 118.8 . . ? C5 C4 C3 119.86(17) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 C6 120.59(17) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C5 C6 C1 118.74(16) . . ? C5 C6 C7 120.37(16) . . ? C1 C6 C7 120.85(15) . . ? C8 C7 C12 119.45(16) . . ? C8 C7 C6 117.92(15) . . ? C12 C7 C6 122.54(16) . . ? C9 C8 C7 120.98(17) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C8 C9 C10 119.95(17) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C9 C10 C11 120.70(17) . . ? C9 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C10 C11 C12 119.67(16) . . ? C10 C11 C13 117.56(16) . . ? C12 C11 C13 122.72(15) . . ? C7 C12 C11 118.42(15) . . ? C7 C12 Cr1 120.44(12) . . ? C11 C12 Cr1 120.76(12) . . ? C18 C13 C14 119.17(15) . . ? C18 C13 C11 120.64(15) . . ? C14 C13 C11 120.18(16) . . ? C15 C14 C13 120.64(16) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C14 C15 C16 119.69(16) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C15 C16 C17 122.69(16) . . ? C15 C16 H16A 118.7 . . ? C17 C16 H16A 118.7 . . ? C16 C17 C18 116.70(16) . . ? C16 C17 C23 121.64(15) . . ? C18 C17 C23 121.64(15) . . ? O2 C18 C13 119.61(15) . . ? O2 C18 C17 119.31(15) . . ? C13 C18 C17 121.07(15) . . ? C2 C19 C21 109.56(14) . . ? C2 C19 C22 112.21(15) . . ? C21 C19 C22 107.03(14) . . ? C2 C19 C20 110.35(14) . . ? C21 C19 C20 110.64(14) . . ? C22 C19 C20 106.98(15) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C17 C23 C24 112.44(14) . . ? C17 C23 C25 108.86(14) . . ? C24 C23 C25 107.75(14) . . ? C17 C23 C26 110.33(14) . . ? C24 C23 C26 106.58(14) . . ? C25 C23 C26 110.84(14) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? P1 C27 Cr1 120.32(9) . . ? P1 C27 H27B 109.5(11) . . ? Cr1 C27 H27B 101.8(11) . . ? P1 C27 H27A 108.2(11) . . ? Cr1 C27 H27A 107.2(11) . . ? H27B C27 H27A 109.5(16) . . ? C33 C28 C29 119.55(16) . . ? C33 C28 P1 121.33(13) . . ? C29 C28 P1 118.97(13) . . ? C30 C29 C28 120.07(16) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C31 120.09(17) . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C32 C31 C30 120.17(17) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C31 C32 C33 120.11(17) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C32 C33 C28 120.00(16) . . ? C32 C33 H33A 120.0 . . ? C28 C33 H33A 120.0 . . ? C35 C34 C39 119.30(15) . . ? C35 C34 P1 121.67(13) . . ? C39 C34 P1 119.03(13) . . ? C34 C35 C36 120.02(16) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C37 C36 C35 120.12(17) . . ? C37 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C36 C37 C38 120.30(16) . . ? C36 C37 H37A 119.8 . . ? C38 C37 H37A 119.8 . . ? C39 C38 C37 119.72(16) . . ? C39 C38 H38A 120.1 . . ? C37 C38 H38A 120.1 . . ? C38 C39 C34 120.53(16) . . ? C38 C39 H39A 119.7 . . ? C34 C39 H39A 119.7 . . ? C45 C40 C41 119.49(16) . . ? C45 C40 P1 123.71(14) . . ? C41 C40 P1 116.78(13) . . ? C42 C41 C40 120.15(17) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C41 C42 C43 119.94(18) . . ? C41 C42 H42A 120.0 . . ? C43 C42 H42A 120.0 . . ? C44 C43 C42 119.98(17) . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C43 C44 C45 120.86(17) . . ? C43 C44 H44A 119.6 . . ? C45 C44 H44A 119.6 . . ? C44 C45 C40 119.56(17) . . ? C44 C45 H45A 120.2 . . ? C40 C45 H45A 120.2 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C52 117.9(2) . . ? C48 C47 C46 120.6(2) . . ? C52 C47 C46 121.5(2) . . ? C47 C48 C49 120.7(2) . . ? C47 C48 H48A 119.6 . . ? C49 C48 H48A 119.6 . . ? C50 C49 C48 120.7(2) . . ? C50 C49 H49A 119.6 . . ? C48 C49 H49A 119.6 . . ? C49 C50 C51 119.0(2) . . ? C49 C50 H50A 120.5 . . ? C51 C50 H50A 120.5 . . ? C50 C51 C52 120.4(2) . . ? C50 C51 H51A 119.8 . . ? C52 C51 H51A 119.8 . . ? C51 C52 C47 121.2(2) . . ? C51 C52 H52A 119.4 . . ? C47 C52 H52A 119.4 . . ? C54 C53 H53A 109.5 . . ? C54 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C54 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C59 C54 C55 117.87(19) . . ? C59 C54 C53 120.73(18) . . ? C55 C54 C53 121.38(18) . . ? C56 C55 C54 120.98(18) . . ? C56 C55 H55A 119.5 . . ? C54 C55 H55A 119.5 . . ? C57 C56 C55 120.30(19) . . ? C57 C56 H56A 119.9 . . ? C55 C56 H56A 119.9 . . ? C58 C57 C56 119.1(2) . . ? C58 C57 H57A 120.4 . . ? C56 C57 H57A 120.4 . . ? C57 C58 C59 120.75(19) . . ? C57 C58 H58A 119.6 . . ? C59 C58 H58A 119.6 . . ? C58 C59 C54 120.92(19) . . ? C58 C59 H59A 119.5 . . ? C54 C59 H59A 119.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.482 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.052