Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Connelly, N.' 'Adams, Christopher J.' 'Bartlett, Ian M.' 'Harding, David J.' 'Hayward, Owen D.' 'Martin, Antonio J.' 'Orpen, A.' 'Quayle, Michael J.' 'Rieger, P.' _publ_contact_author_name 'Prof N Connelly' _publ_contact_author_address ; Prof N Connelly School of Chemistry University of Bristol Bristol BS8 1TS UNITED KINGDOM ; _publ_contact_author_email 'NEIL.CONNELLY@BRISTOL.AC.UK' _publ_section_title ; Redox routes to arenechromium complexes of two-, three- and four-electron alkynes; structure and bonding in paramagnetic [Cr(CO)L( - RC CR)( -arene)]+ ; data_1 _database_code_CSD 189051 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H26 Cr O2' _chemical_formula_weight 434.48 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' '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1132(14) _cell_length_b 9.353(3) _cell_length_c 16.781(3) _cell_angle_alpha 88.5(2) _cell_angle_beta 81.84(16) _cell_angle_gamma 72.0(2) _cell_volume 1050.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 0.566 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.546 _exptl_absorpt_correction_T_max 0.627 _exptl_absorpt_process_details 'XPREP' _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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4987 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3518 _reflns_number_gt 3332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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. ; _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^)+(0.0337P)^2^+0.7740P] 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 SHELXL _refine_ls_extinction_coef 0.0063(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3518 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.67583(4) 0.40516(3) 0.272261(15) 0.01586(10) Uani 1 1 d . . . C1 C 0.3882(3) 0.3369(2) 0.28350(12) 0.0241(4) Uani 1 1 d . . . C2 C 0.3870(3) 0.4228(2) 0.35108(11) 0.0241(4) Uani 1 1 d . . . H2 H 0.3725 0.3815 0.4031 0.029 Uiso 1 1 calc R . . C3 C 0.4066(2) 0.5683(2) 0.34430(11) 0.0222(4) Uani 1 1 d . . . C4 C 0.4335(2) 0.62759(19) 0.26743(11) 0.0211(4) Uani 1 1 d . . . C5 C 0.4420(2) 0.5398(2) 0.19767(10) 0.0216(4) Uani 1 1 d . . . C6 C 0.4177(2) 0.3949(2) 0.20573(11) 0.0227(4) Uani 1 1 d . . . C7 C 0.3515(3) 0.1866(2) 0.29575(15) 0.0368(5) Uani 1 1 d . . . H7C H 0.4600 0.1087 0.2643 0.055 Uiso 1 1 calc R . . H7B H 0.2242 0.1917 0.2780 0.055 Uiso 1 1 calc R . . H7A H 0.3466 0.1618 0.3530 0.055 Uiso 1 1 calc R . . C9 C 0.3934(3) 0.6579(2) 0.41978(12) 0.0328(5) Uani 1 1 d . . . H9C H 0.3777 0.5969 0.4671 0.049 Uiso 1 1 calc R . . H9B H 0.2781 0.7492 0.4225 0.049 Uiso 1 1 calc R . . H9A H 0.5157 0.6857 0.4186 0.049 Uiso 1 1 calc R . . C10 C 0.4507(3) 0.7848(2) 0.25961(13) 0.0297(4) Uani 1 1 d . . . H10C H 0.3172 0.8578 0.2614 0.045 Uiso 1 1 calc R . . H10B H 0.5317 0.7924 0.2083 0.045 Uiso 1 1 calc R . . H10A H 0.5144 0.8059 0.3041 0.045 Uiso 1 1 calc R . . C11 C 0.4571(3) 0.6091(2) 0.11547(12) 0.0324(4) Uani 1 1 d . . . H11C H 0.5526 0.6661 0.1122 0.049 Uiso 1 1 calc R . . H11B H 0.3257 0.6767 0.1070 0.049 Uiso 1 1 calc R . . H11A H 0.5029 0.5293 0.0739 0.049 Uiso 1 1 calc R . . C12 C 0.4199(3) 0.3023(2) 0.13278(13) 0.0356(5) Uani 1 1 d . . . H12F H 0.5069 0.3258 0.0871 0.053 Uiso 0.50 1 calc PR . . H12E H 0.2840 0.3260 0.1194 0.053 Uiso 0.50 1 calc PR . . H12D H 0.4703 0.1951 0.1447 0.053 Uiso 0.50 1 calc PR . . H12C H 0.3339 0.2388 0.1470 0.053 Uiso 0.50 1 calc PR . . H12B H 0.5567 0.2386 0.1147 0.053 Uiso 0.50 1 calc PR . . H12A H 0.3705 0.3695 0.0894 0.053 Uiso 0.50 1 calc PR . . C13 C 0.8180(3) 0.16763(19) 0.26986(10) 0.0195(4) Uani 1 1 d . . . C21 C 0.8313(2) 0.04557(19) 0.32655(10) 0.0200(4) Uani 1 1 d . . . C22 C 0.8954(3) -0.1045(2) 0.29911(11) 0.0232(4) Uani 1 1 d . . . H22 H 0.9308 -0.1264 0.2430 0.028 Uiso 1 1 calc R . . C23 C 0.9078(3) -0.2211(2) 0.35260(12) 0.0274(4) Uani 1 1 d . . . H23 H 0.9520 -0.3221 0.3329 0.033 Uiso 1 1 calc R . . C24 C 0.8563(3) -0.1917(2) 0.43487(12) 0.0313(4) Uani 1 1 d . . . H24 H 0.8655 -0.2719 0.4715 0.038 Uiso 1 1 calc R . . C25 C 0.7915(4) -0.0446(2) 0.46277(12) 0.0374(5) Uani 1 1 d . . . H25 H 0.7563 -0.0236 0.5190 0.045 Uiso 1 1 calc R . . C26 C 0.7773(3) 0.0736(2) 0.40937(11) 0.0320(4) Uani 1 1 d . . . H26 H 0.7303 0.1743 0.4295 0.038 Uiso 1 1 calc R . . C14 C 0.8601(2) 0.21333(18) 0.20041(10) 0.0185(3) Uani 1 1 d . . . C27 C 0.9741(2) 0.18242(19) 0.11996(10) 0.0186(3) Uani 1 1 d . . . C28 C 0.9465(3) 0.2899(2) 0.05958(10) 0.0234(4) Uani 1 1 d . . . H28 H 0.8489 0.3855 0.0704 0.028 Uiso 1 1 calc R . . C29 C 1.0601(3) 0.2585(2) -0.01620(11) 0.0296(4) Uani 1 1 d . . . H29 H 1.0387 0.3321 -0.0568 0.036 Uiso 1 1 calc R . . C30 C 1.2041(3) 0.1201(2) -0.03245(11) 0.0323(5) Uani 1 1 d . . . H30 H 1.2821 0.0990 -0.0841 0.039 Uiso 1 1 calc R . . C31 C 1.2346(3) 0.0123(2) 0.02681(12) 0.0301(4) Uani 1 1 d . . . H31 H 1.3339 -0.0825 0.0159 0.036 Uiso 1 1 calc R . . C32 C 1.1198(3) 0.0431(2) 0.10195(11) 0.0240(4) Uani 1 1 d . . . H32 H 1.1404 -0.0317 0.1420 0.029 Uiso 1 1 calc R . . C15 C 0.8155(3) 0.40846(19) 0.35486(10) 0.0205(4) Uani 1 1 d . . . O1 O 0.9058(2) 0.41660(16) 0.40647(8) 0.0309(3) Uani 1 1 d . . . C16 C 0.8532(3) 0.49214(19) 0.22040(10) 0.0197(4) Uani 1 1 d . . . O2 O 0.9652(2) 0.55202(15) 0.18956(8) 0.0291(3) 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 0.01608(16) 0.01483(15) 0.01602(16) 0.00001(10) -0.00133(10) -0.00423(11) C1 0.0143(8) 0.0216(9) 0.0364(10) 0.0003(8) -0.0016(7) -0.0064(7) C2 0.0175(9) 0.0276(10) 0.0245(9) 0.0033(7) 0.0027(7) -0.0056(7) C3 0.0149(8) 0.0237(9) 0.0245(9) -0.0052(7) -0.0005(7) -0.0016(7) C4 0.0145(8) 0.0181(9) 0.0289(9) -0.0003(7) -0.0038(7) -0.0023(7) C5 0.0155(8) 0.0237(9) 0.0235(9) 0.0014(7) -0.0050(7) -0.0020(7) C6 0.0151(8) 0.0236(9) 0.0291(9) -0.0061(7) -0.0051(7) -0.0043(7) C7 0.0297(11) 0.0261(10) 0.0582(14) 0.0035(9) -0.0052(9) -0.0143(8) C9 0.0280(10) 0.0373(11) 0.0279(10) -0.0124(8) -0.0012(8) -0.0026(8) C10 0.0295(10) 0.0183(9) 0.0411(11) 0.0022(8) -0.0089(8) -0.0055(8) C11 0.0330(11) 0.0352(11) 0.0260(10) 0.0063(8) -0.0075(8) -0.0052(9) C12 0.0280(10) 0.0407(12) 0.0400(12) -0.0160(9) -0.0067(9) -0.0110(9) C13 0.0197(8) 0.0161(8) 0.0213(9) -0.0027(7) -0.0030(7) -0.0031(7) C21 0.0187(8) 0.0203(9) 0.0209(9) 0.0022(7) -0.0024(7) -0.0064(7) C22 0.0217(9) 0.0225(9) 0.0246(9) -0.0007(7) -0.0020(7) -0.0062(7) C23 0.0262(10) 0.0185(9) 0.0389(11) 0.0034(8) -0.0079(8) -0.0078(7) C24 0.0357(11) 0.0278(10) 0.0349(11) 0.0146(8) -0.0123(9) -0.0145(8) C25 0.0569(14) 0.0355(12) 0.0221(10) 0.0067(8) -0.0037(9) -0.0190(10) C26 0.0487(12) 0.0227(10) 0.0235(10) 0.0011(8) -0.0005(8) -0.0116(9) C14 0.0178(8) 0.0168(8) 0.0204(9) -0.0009(6) -0.0035(6) -0.0041(6) C27 0.0184(8) 0.0218(9) 0.0168(8) -0.0008(7) -0.0018(6) -0.0079(7) C28 0.0249(9) 0.0249(9) 0.0213(9) 0.0017(7) -0.0044(7) -0.0085(7) C29 0.0363(11) 0.0382(11) 0.0188(9) 0.0053(8) -0.0046(8) -0.0179(9) C30 0.0350(11) 0.0441(12) 0.0199(9) -0.0070(8) 0.0070(8) -0.0195(9) C31 0.0258(10) 0.0310(10) 0.0303(10) -0.0086(8) 0.0037(8) -0.0070(8) C32 0.0240(9) 0.0236(9) 0.0236(9) 0.0004(7) -0.0017(7) -0.0069(7) C15 0.0218(9) 0.0167(8) 0.0209(9) 0.0013(7) 0.0011(7) -0.0048(7) O1 0.0355(8) 0.0363(8) 0.0249(7) 0.0039(6) -0.0117(6) -0.0140(6) C16 0.0221(9) 0.0183(8) 0.0159(8) -0.0003(6) -0.0044(7) -0.0015(7) O2 0.0290(7) 0.0344(7) 0.0274(7) 0.0060(6) -0.0006(5) -0.0170(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C16 1.816(4) . ? Cr1 C15 1.823(3) . ? Cr1 C13 2.136(4) . ? Cr1 C14 2.144(6) . ? Cr1 C2 2.242(4) . ? Cr1 C3 2.255(7) . ? Cr1 C4 2.262(6) . ? Cr1 C5 2.265(5) . ? Cr1 C1 2.307(3) . ? Cr1 C6 2.307(3) . ? C1 C2 1.404(4) . ? C1 C6 1.413(3) . ? C1 C7 1.511(3) . ? C2 C3 1.411(3) . ? C3 C4 1.402(3) . ? C3 C9 1.512(4) . ? C4 C5 1.431(4) . ? C4 C10 1.514(3) . ? C5 C6 1.419(3) . ? C5 C11 1.513(3) . ? C6 C12 1.513(4) . ? C13 C14 1.259(3) . ? C13 C21 1.456(4) . ? C21 C26 1.397(3) . ? C21 C22 1.403(4) . ? C22 C23 1.384(4) . ? C23 C24 1.389(3) . ? C24 C25 1.380(4) . ? C25 C26 1.393(4) . ? C14 C27 1.459(3) . ? C27 C32 1.399(5) . ? C27 C28 1.399(4) . ? C28 C29 1.392(4) . ? C29 C30 1.384(5) . ? C30 C31 1.388(4) . ? C31 C32 1.386(4) . ? C15 O1 1.166(3) . ? C16 O2 1.166(3) . ? 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 C16 Cr1 C15 81.50(13) . . ? C16 Cr1 C13 107.91(19) . . ? C15 Cr1 C13 85.3(2) . . ? C16 Cr1 C14 82.47(14) . . ? C15 Cr1 C14 103.9(2) . . ? C13 Cr1 C14 34.22(13) . . ? C16 Cr1 C2 150.60(11) . . ? C15 Cr1 C2 95.38(10) . . ? C13 Cr1 C2 100.9(3) . . ? C14 Cr1 C2 126.26(17) . . ? C16 Cr1 C3 114.04(11) . . ? C15 Cr1 C3 88.33(17) . . ? C13 Cr1 C3 136.03(18) . . ? C14 Cr1 C3 161.05(10) . . ? C2 Cr1 C3 36.57(11) . . ? C16 Cr1 C4 88.37(15) . . ? C15 Cr1 C4 110.1(2) . . ? C13 Cr1 C4 159.46(10) . . ? C14 Cr1 C4 143.00(13) . . ? C2 Cr1 C4 65.1(2) . . ? C3 Cr1 C4 36.18(14) . . ? C16 Cr1 C5 89.79(14) . . ? C15 Cr1 C5 146.36(11) . . ? C13 Cr1 C5 128.17(19) . . ? C14 Cr1 C5 107.05(18) . . ? C2 Cr1 C5 76.65(15) . . ? C3 Cr1 C5 65.66(16) . . ? C4 Cr1 C5 36.85(14) . . ? C16 Cr1 C1 152.75(10) . . ? C15 Cr1 C1 124.91(13) . . ? C13 Cr1 C1 83.3(2) . . ? C14 Cr1 C1 95.68(16) . . ? C2 Cr1 C1 35.91(10) . . ? C3 Cr1 C1 65.37(12) . . ? C4 Cr1 C1 76.77(13) . . ? C5 Cr1 C1 64.63(13) . . ? C16 Cr1 C6 117.23(12) . . ? C15 Cr1 C6 159.75(9) . . ? C13 Cr1 C6 95.3(2) . . ? C14 Cr1 C6 87.06(19) . . ? C2 Cr1 C6 64.59(7) . . ? C3 Cr1 C6 77.22(15) . . ? C4 Cr1 C6 65.56(17) . . ? C5 Cr1 C6 36.14(9) . . ? C1 Cr1 C6 35.68(9) . . ? C2 C1 C6 119.29(17) . . ? C2 C1 C7 119.2(2) . . ? C6 C1 C7 121.5(3) . . ? C2 C1 Cr1 69.53(19) . . ? C6 C1 Cr1 72.16(18) . . ? C7 C1 Cr1 132.1(2) . . ? C1 C2 C3 122.1(2) . . ? C1 C2 Cr1 74.55(19) . . ? C3 C2 Cr1 72.2(3) . . ? C4 C3 C2 118.9(2) . . ? C4 C3 C9 121.63(17) . . ? C2 C3 C9 119.4(2) . . ? C4 C3 Cr1 72.2(2) . . ? C2 C3 Cr1 71.2(2) . . ? C9 C3 Cr1 129.38(19) . . ? C3 C4 C5 119.75(17) . . ? C3 C4 C10 119.3(2) . . ? C5 C4 C10 120.9(2) . . ? C3 C4 Cr1 71.7(2) . . ? C5 C4 Cr1 71.7(2) . . ? C10 C4 Cr1 129.40(15) . . ? C6 C5 C4 120.5(2) . . ? C6 C5 C11 120.1(2) . . ? C4 C5 C11 119.11(17) . . ? C6 C5 Cr1 73.6(2) . . ? C4 C5 Cr1 71.45(19) . . ? C11 C5 Cr1 132.45(17) . . ? C1 C6 C5 119.3(2) . . ? C1 C6 C12 119.38(18) . . ? C5 C6 C12 121.3(2) . . ? C1 C6 Cr1 72.16(16) . . ? C5 C6 Cr1 70.3(2) . . ? C12 C6 Cr1 130.3(2) . . ? C14 C13 C21 150.3(2) . . ? C14 C13 Cr1 73.3(3) . . ? C21 C13 Cr1 136.45(17) . . ? C26 C21 C22 117.9(3) . . ? C26 C21 C13 121.5(2) . . ? C22 C21 C13 120.61(18) . . ? C23 C22 C21 121.0(2) . . ? C22 C23 C24 120.5(2) . . ? C25 C24 C23 119.3(3) . . ? C24 C25 C26 120.7(2) . . ? C25 C26 C21 120.7(2) . . ? C13 C14 C27 149.08(19) . . ? C13 C14 Cr1 72.53(19) . . ? C27 C14 Cr1 138.0(2) . . ? C32 C27 C28 118.0(2) . . ? C32 C27 C14 120.0(3) . . ? C28 C27 C14 122.0(2) . . ? C29 C28 C27 120.8(2) . . ? C30 C29 C28 120.1(3) . . ? C29 C30 C31 119.9(2) . . ? C32 C31 C30 119.9(3) . . ? C31 C32 C27 121.2(3) . . ? O1 C15 Cr1 176.99(15) . . ? O2 C16 Cr1 177.35(15) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.224 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.045 #===END data_1plus _database_code_CSD 189052 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 Cl2 Cr F6 O2 P' _chemical_formula_weight 664.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.1866(19) _cell_length_b 15.768(3) _cell_length_c 9.913(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.83(16) _cell_angle_gamma 90.00 _cell_volume 1410.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 678 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.300 _exptl_absorpt_correction_T_max 0.407 _exptl_absorpt_process_details 'XPREP' _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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 6858 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.11 _reflns_number_total 3808 _reflns_number_gt 3243 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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. ; _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^)+(0.0518P)^2^+2.8675P] 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 SHELXL _refine_ls_extinction_coef 0.0013(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(4) _refine_ls_number_reflns 3808 _refine_ls_number_parameters 362 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _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 0.04743(9) 0.20514(7) 0.69014(9) 0.0199(2) Uani 1 1 d . . . C1 C 0.2503(7) 0.1356(4) 0.6395(6) 0.0235(14) Uani 1 1 d . . . C2 C 0.1943(7) 0.1936(5) 0.5347(6) 0.0252(14) Uani 1 1 d . . . H2A H 0.2565 0.2430 0.5176 0.030 Uiso 1 1 calc R . . C3 C 0.0457(6) 0.1871(4) 0.4609(6) 0.0219(14) Uani 1 1 d . . . C4 C -0.0472(7) 0.1262(5) 0.5025(7) 0.0254(15) Uani 1 1 d . . . C5 C 0.0068(7) 0.0701(5) 0.6148(7) 0.0270(16) Uani 1 1 d . . . C6 C 0.1568(7) 0.0742(4) 0.6800(7) 0.0256(15) Uani 1 1 d . . . C7 C -0.0014(8) 0.2468(5) 0.3410(7) 0.0357(18) Uani 1 1 d . . . H7A H 0.0123 0.2190 0.2559 0.054 Uiso 1 1 calc R . . H7B H 0.0589 0.2984 0.3551 0.054 Uiso 1 1 calc R . . H7C H -0.1061 0.2616 0.3344 0.054 Uiso 1 1 calc R . . C8 C -0.2056(7) 0.1181(6) 0.4222(8) 0.041(2) Uani 1 1 d . . . H8A H -0.2077 0.0782 0.3462 0.061 Uiso 1 1 calc R . . H8B H -0.2407 0.1737 0.3856 0.061 Uiso 1 1 calc R . . H8C H -0.2701 0.0973 0.4833 0.061 Uiso 1 1 calc R . . C9 C -0.0957(9) 0.0027(5) 0.6538(8) 0.043(2) Uani 1 1 d . . . H9A H -0.0868 -0.0492 0.6016 0.064 Uiso 1 1 calc R . . H9B H -0.1982 0.0232 0.6325 0.064 Uiso 1 1 calc R . . H9C H -0.0684 -0.0092 0.7523 0.064 Uiso 1 1 calc R . . C10 C 0.2186(9) 0.0092(5) 0.7873(8) 0.0399(19) Uani 1 1 d . . . H10A H 0.2564 -0.0395 0.7429 0.060 Uiso 1 1 calc R . . H10B H 0.1401 -0.0098 0.8350 0.060 Uiso 1 1 calc R . . H10C H 0.2994 0.0345 0.8537 0.060 Uiso 1 1 calc R . . C11 C 0.4099(7) 0.1440(6) 0.7100(8) 0.0404(19) Uani 1 1 d . . . H11A H 0.4716 0.1064 0.6657 0.061 Uiso 1 1 calc R . . H11B H 0.4195 0.1283 0.8069 0.061 Uiso 1 1 calc R . . H11C H 0.4423 0.2028 0.7032 0.061 Uiso 1 1 calc R . . C13 C 0.1253(6) 0.2041(6) 0.8962(6) 0.0264(13) Uani 1 1 d . . . C21 C 0.1351(7) 0.1508(5) 1.0180(6) 0.0242(15) Uani 1 1 d . . . C22 C 0.0298(8) 0.0905(5) 1.0349(7) 0.0326(17) Uani 1 1 d . . . H22A H -0.0551 0.0834 0.9645 0.039 Uiso 1 1 calc R . . C23 C 0.0449(8) 0.0410(5) 1.1507(7) 0.0327(16) Uani 1 1 d . . . H23A H -0.0306 0.0020 1.1620 0.039 Uiso 1 1 calc R . . C24 C 0.1746(8) 0.0488(5) 1.2532(7) 0.0332(17) Uani 1 1 d . . . H24A H 0.1887 0.0132 1.3318 0.040 Uiso 1 1 calc R . . C25 C 0.2798(8) 0.1085(5) 1.2381(7) 0.0288(16) Uani 1 1 d . . . H25A H 0.3661 0.1145 1.3072 0.035 Uiso 1 1 calc R . . C26 C 0.2604(7) 0.1594(5) 1.1232(7) 0.0289(16) Uani 1 1 d . . . H26A H 0.3329 0.2010 1.1148 0.035 Uiso 1 1 calc R . . C14 C 0.1706(7) 0.2714(5) 0.8488(6) 0.0244(15) Uani 1 1 d . . . C27 C 0.2546(7) 0.3505(4) 0.8804(6) 0.0259(14) Uani 1 1 d . . . C28 C 0.3254(7) 0.3870(5) 0.7812(7) 0.0318(16) Uani 1 1 d . . . H28A H 0.3185 0.3614 0.6935 0.038 Uiso 1 1 calc R . . C29 C 0.4066(8) 0.4617(5) 0.8134(9) 0.043(2) Uani 1 1 d . . . H29A H 0.4564 0.4869 0.7477 0.052 Uiso 1 1 calc R . . C30 C 0.4143(8) 0.4979(5) 0.9371(9) 0.044(2) Uani 1 1 d . . . H30A H 0.4693 0.5488 0.9572 0.053 Uiso 1 1 calc R . . C31 C 0.3452(9) 0.4635(5) 1.0347(9) 0.043(2) Uani 1 1 d . . . H31A H 0.3521 0.4904 1.1214 0.051 Uiso 1 1 calc R . . C32 C 0.2644(7) 0.3886(5) 1.0065(7) 0.0315(16) Uani 1 1 d . . . H32A H 0.2164 0.3641 1.0740 0.038 Uiso 1 1 calc R . . C15 C -0.1392(7) 0.1948(6) 0.7402(6) 0.0314(17) Uani 1 1 d . . . O1 O -0.2526(5) 0.1829(4) 0.7676(5) 0.0490(17) Uani 1 1 d . . . C16 C 0.0112(7) 0.3186(5) 0.6402(7) 0.0236(16) Uani 1 1 d . . . O2 O -0.0063(6) 0.3876(4) 0.6101(5) 0.0362(12) Uani 1 1 d . . . P1 P 0.5406(2) 0.35864(15) 1.4445(2) 0.0396(5) Uani 1 1 d . . . F1 F 0.5804(7) 0.3447(5) 1.6051(5) 0.088(2) Uani 1 1 d . . . F2 F 0.5036(7) 0.3723(6) 1.2878(6) 0.106(3) Uani 1 1 d . . . F3 F 0.7081(5) 0.3434(5) 1.4352(6) 0.084(2) Uani 1 1 d . . . F4 F 0.5711(9) 0.4557(4) 1.4662(8) 0.102(2) Uani 1 1 d . . . F5 F 0.5096(7) 0.2599(4) 1.4251(8) 0.091(2) Uani 1 1 d . . . F6 F 0.3716(5) 0.3710(4) 1.4573(6) 0.0766(18) Uani 1 1 d . . . C50 C -0.3324(10) 0.3177(6) 1.0010(11) 0.063(3) Uani 1 1 d . . . H50A H -0.3704 0.3597 1.0602 0.076 Uiso 1 1 calc R . . H50B H -0.3927 0.3222 0.9074 0.076 Uiso 1 1 calc R . . Cl1 Cl -0.3490(2) 0.21618(18) 1.0648(2) 0.0572(6) Uani 1 1 d . . . Cl2 Cl -0.1421(2) 0.34092(14) 0.9957(2) 0.0535(6) 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 0.0167(4) 0.0209(5) 0.0218(4) -0.0029(5) 0.0026(3) -0.0007(5) C1 0.020(3) 0.022(4) 0.030(3) -0.008(3) 0.007(3) -0.001(3) C2 0.030(3) 0.023(4) 0.024(3) 0.002(3) 0.007(2) 0.000(3) C3 0.028(3) 0.017(4) 0.023(3) -0.003(2) 0.009(2) 0.003(3) C4 0.018(3) 0.033(4) 0.025(3) -0.015(3) 0.003(3) 0.003(3) C5 0.026(3) 0.023(4) 0.035(4) -0.011(3) 0.013(3) -0.006(3) C6 0.030(3) 0.018(4) 0.027(3) 0.000(3) 0.002(3) 0.010(3) C7 0.040(4) 0.044(5) 0.022(3) -0.002(3) 0.002(3) 0.006(4) C8 0.021(3) 0.057(6) 0.040(4) -0.010(4) -0.004(3) -0.012(4) C9 0.046(4) 0.037(5) 0.051(5) -0.010(4) 0.024(4) -0.013(4) C10 0.050(5) 0.032(5) 0.041(4) 0.012(3) 0.016(4) 0.015(4) C11 0.022(3) 0.046(5) 0.051(5) -0.003(4) 0.002(3) 0.005(3) C13 0.025(3) 0.028(4) 0.026(3) -0.006(4) 0.006(2) -0.005(4) C21 0.020(3) 0.031(4) 0.022(3) -0.002(3) 0.003(2) -0.003(3) C22 0.032(4) 0.036(5) 0.029(4) -0.003(3) 0.005(3) -0.005(3) C23 0.039(4) 0.028(4) 0.033(4) -0.003(3) 0.011(3) -0.004(3) C24 0.040(4) 0.031(4) 0.028(4) -0.002(3) 0.004(3) 0.007(3) C25 0.028(3) 0.030(4) 0.026(3) 0.001(3) -0.002(3) 0.008(3) C26 0.026(3) 0.032(4) 0.028(4) 0.001(3) 0.004(3) -0.001(3) C14 0.020(3) 0.029(4) 0.024(3) 0.001(3) 0.003(3) 0.004(3) C27 0.021(3) 0.022(4) 0.031(3) -0.001(3) -0.003(3) 0.000(3) C28 0.028(4) 0.034(4) 0.031(4) 0.004(3) -0.001(3) -0.007(3) C29 0.033(4) 0.032(5) 0.059(5) 0.017(4) -0.006(4) -0.006(4) C30 0.030(4) 0.024(4) 0.071(6) 0.005(4) -0.011(4) -0.008(4) C31 0.040(4) 0.031(5) 0.049(5) -0.010(4) -0.014(4) 0.005(4) C32 0.029(4) 0.031(4) 0.032(4) -0.001(3) -0.002(3) 0.004(3) C15 0.027(3) 0.044(5) 0.023(3) -0.004(3) 0.004(2) 0.012(4) O1 0.024(3) 0.077(5) 0.047(3) -0.015(3) 0.010(2) -0.008(3) C16 0.024(3) 0.027(4) 0.019(3) -0.009(3) 0.003(3) -0.004(3) O2 0.043(3) 0.028(3) 0.034(3) 0.001(2) -0.002(2) 0.004(3) P1 0.0298(10) 0.0481(15) 0.0420(11) 0.0093(10) 0.0096(8) 0.0007(9) F1 0.096(4) 0.121(6) 0.050(3) 0.016(4) 0.018(3) 0.017(4) F2 0.083(4) 0.186(9) 0.046(3) 0.035(4) 0.004(3) -0.002(5) F3 0.032(3) 0.128(6) 0.092(4) -0.004(4) 0.014(3) -0.002(3) F4 0.119(6) 0.053(4) 0.141(6) -0.001(4) 0.043(5) -0.018(4) F5 0.078(4) 0.059(4) 0.143(6) -0.011(4) 0.035(4) -0.007(3) F6 0.040(3) 0.089(5) 0.104(4) 0.025(4) 0.023(3) 0.022(3) C50 0.043(5) 0.046(6) 0.096(8) -0.016(5) 0.001(5) 0.013(4) Cl1 0.0496(11) 0.0719(18) 0.0494(10) 0.0017(12) 0.0075(9) -0.0189(13) Cl2 0.0575(13) 0.0430(14) 0.0645(13) -0.0125(11) 0.0228(10) -0.0101(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C16 1.869(8) . ? Cr1 C15 1.880(6) . ? Cr1 C13 2.034(6) . ? Cr1 C14 2.044(7) . ? Cr1 C2 2.238(6) . ? Cr1 C5 2.264(8) . ? Cr1 C4 2.270(7) . ? Cr1 C3 2.288(6) . ? Cr1 C1 2.298(7) . ? Cr1 C6 2.306(7) . ? C1 C6 1.402(10) . ? C1 C2 1.406(9) . ? C1 C11 1.507(9) . ? C2 C3 1.426(9) . ? C3 C4 1.398(9) . ? C3 C7 1.514(9) . ? C4 C5 1.436(11) . ? C4 C8 1.528(9) . ? C5 C6 1.409(9) . ? C5 C9 1.517(10) . ? C6 C10 1.510(10) . ? C13 C14 1.262(10) . ? C13 C21 1.460(10) . ? C21 C22 1.389(10) . ? C21 C26 1.407(9) . ? C22 C23 1.373(10) . ? C23 C24 1.418(10) . ? C24 C25 1.377(11) . ? C25 C26 1.377(10) . ? C14 C27 1.469(10) . ? C27 C32 1.375(9) . ? C27 C28 1.401(9) . ? C28 C29 1.399(11) . ? C29 C30 1.341(12) . ? C30 C31 1.366(12) . ? C31 C32 1.394(11) . ? C15 O1 1.140(8) . ? C16 O2 1.131(9) . ? P1 F2 1.542(6) . ? P1 F4 1.563(7) . ? P1 F3 1.577(5) . ? P1 F1 1.580(6) . ? P1 F5 1.588(7) . ? P1 F6 1.593(5) . ? C50 Cl1 1.739(11) . ? C50 Cl2 1.796(10) . ? 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 C16 Cr1 C15 91.5(4) . . ? C16 Cr1 C13 106.5(3) . . ? C15 Cr1 C13 84.3(3) . . ? C16 Cr1 C14 76.1(3) . . ? C15 Cr1 C14 104.0(3) . . ? C13 Cr1 C14 36.1(3) . . ? C16 Cr1 C2 89.8(3) . . ? C15 Cr1 C2 150.8(3) . . ? C13 Cr1 C2 123.2(2) . . ? C14 Cr1 C2 104.7(3) . . ? C16 Cr1 C5 143.4(3) . . ? C15 Cr1 C5 84.5(3) . . ? C13 Cr1 C5 109.2(3) . . ? C14 Cr1 C5 140.1(3) . . ? C2 Cr1 C5 77.3(3) . . ? C16 Cr1 C4 106.6(3) . . ? C15 Cr1 C4 86.6(3) . . ? C13 Cr1 C4 145.8(3) . . ? C14 Cr1 C4 169.1(2) . . ? C2 Cr1 C4 65.1(2) . . ? C5 Cr1 C4 36.9(3) . . ? C16 Cr1 C3 83.6(3) . . ? C15 Cr1 C3 114.5(3) . . ? C13 Cr1 C3 158.8(2) . . ? C14 Cr1 C3 136.7(3) . . ? C2 Cr1 C3 36.7(2) . . ? C5 Cr1 C3 65.5(3) . . ? C4 Cr1 C3 35.7(2) . . ? C16 Cr1 C1 120.7(3) . . ? C15 Cr1 C1 146.5(3) . . ? C13 Cr1 C1 94.0(3) . . ? C14 Cr1 C1 93.3(3) . . ? C2 Cr1 C1 36.1(2) . . ? C5 Cr1 C1 64.5(3) . . ? C4 Cr1 C1 76.2(2) . . ? C3 Cr1 C1 65.0(3) . . ? C16 Cr1 C6 154.5(3) . . ? C15 Cr1 C6 111.1(3) . . ? C13 Cr1 C6 87.9(3) . . ? C14 Cr1 C6 108.0(3) . . ? C2 Cr1 C6 64.7(3) . . ? C5 Cr1 C6 35.9(2) . . ? C4 Cr1 C6 64.9(3) . . ? C3 Cr1 C6 76.5(3) . . ? C1 Cr1 C6 35.5(3) . . ? C6 C1 C2 120.1(6) . . ? C6 C1 C11 121.5(6) . . ? C2 C1 C11 118.3(6) . . ? C6 C1 Cr1 72.6(4) . . ? C2 C1 Cr1 69.7(4) . . ? C11 C1 Cr1 127.9(5) . . ? C1 C2 C3 121.0(6) . . ? C1 C2 Cr1 74.3(4) . . ? C3 C2 Cr1 73.5(3) . . ? C4 C3 C2 118.4(6) . . ? C4 C3 C7 123.9(6) . . ? C2 C3 C7 117.6(6) . . ? C4 C3 Cr1 71.5(4) . . ? C2 C3 Cr1 69.8(4) . . ? C7 C3 Cr1 130.6(4) . . ? C3 C4 C5 120.7(6) . . ? C3 C4 C8 118.6(6) . . ? C5 C4 C8 120.6(7) . . ? C3 C4 Cr1 72.8(4) . . ? C5 C4 Cr1 71.3(4) . . ? C8 C4 Cr1 130.8(5) . . ? C6 C5 C4 119.5(6) . . ? C6 C5 C9 121.1(7) . . ? C4 C5 C9 119.2(6) . . ? C6 C5 Cr1 73.7(4) . . ? C4 C5 Cr1 71.8(4) . . ? C9 C5 Cr1 130.3(5) . . ? C1 C6 C5 120.0(6) . . ? C1 C6 C10 120.1(6) . . ? C5 C6 C10 119.8(7) . . ? C1 C6 Cr1 71.9(4) . . ? C5 C6 Cr1 70.4(4) . . ? C10 C6 Cr1 133.4(5) . . ? C14 C13 C21 145.0(6) . . ? C14 C13 Cr1 72.4(4) . . ? C21 C13 Cr1 142.2(6) . . ? C22 C21 C26 117.9(6) . . ? C22 C21 C13 123.9(6) . . ? C26 C21 C13 118.2(6) . . ? C23 C22 C21 121.7(6) . . ? C22 C23 C24 119.3(7) . . ? C25 C24 C23 119.6(7) . . ? C24 C25 C26 120.2(6) . . ? C25 C26 C21 121.2(7) . . ? C13 C14 C27 146.2(6) . . ? C13 C14 Cr1 71.5(4) . . ? C27 C14 Cr1 142.3(5) . . ? C32 C27 C28 119.9(7) . . ? C32 C27 C14 120.5(6) . . ? C28 C27 C14 119.6(6) . . ? C29 C28 C27 119.0(7) . . ? C30 C29 C28 120.0(8) . . ? C29 C30 C31 121.8(8) . . ? C30 C31 C32 119.6(8) . . ? C27 C32 C31 119.6(7) . . ? O1 C15 Cr1 175.3(8) . . ? O2 C16 Cr1 177.9(6) . . ? F2 P1 F4 90.1(5) . . ? F2 P1 F3 89.7(4) . . ? F4 P1 F3 90.3(4) . . ? F2 P1 F1 179.3(4) . . ? F4 P1 F1 89.8(4) . . ? F3 P1 F1 89.7(4) . . ? F2 P1 F5 90.8(5) . . ? F4 P1 F5 179.0(4) . . ? F3 P1 F5 89.9(4) . . ? F1 P1 F5 89.3(4) . . ? F2 P1 F6 91.7(4) . . ? F4 P1 F6 91.2(4) . . ? F3 P1 F6 177.9(4) . . ? F1 P1 F6 88.9(4) . . ? F5 P1 F6 88.5(4) . . ? Cl1 C50 Cl2 110.5(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.450 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.084 #===END data_3plus _database_code_CSD 189053 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Cr F6 O4 P' _chemical_formula_weight 653.53 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' 'F' 'F' 0.0171 0.0103 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.9707(18) _cell_length_b 18.592(4) _cell_length_c 17.104(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.00(3) _cell_angle_gamma 90.00 _cell_volume 2831.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 197 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 0.536 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.419 _exptl_absorpt_correction_T_max 0.714 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 10012 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 23.28 _reflns_number_total 3920 _reflns_number_gt 3157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. ; _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^)+(0.0546P)^2^+8.7062P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3920 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1442 _refine_ls_wR_factor_gt 0.1312 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 0.23799(7) 0.74034(4) 0.49812(4) 0.0160(2) Uani 1 1 d . . . C1 C 0.2851(5) 0.6617(2) 0.4021(3) 0.0210(11) Uani 1 1 d . . . C2 C 0.1761(5) 0.6305(2) 0.4440(3) 0.0219(11) Uani 1 1 d . . . C3 C 0.0422(5) 0.6696(2) 0.4549(3) 0.0203(10) Uani 1 1 d . . . C4 C 0.0144(5) 0.7367(2) 0.4162(3) 0.0201(10) Uani 1 1 d . . . C5 C 0.1231(5) 0.7684(2) 0.3736(3) 0.0188(10) Uani 1 1 d . . . C6 C 0.2612(5) 0.7316(2) 0.3674(3) 0.0200(10) Uani 1 1 d . . . C7 C 0.4261(6) 0.6200(3) 0.3920(3) 0.0302(12) Uani 1 1 d . . . H7A H 0.4095 0.5913 0.3452 0.045 Uiso 1 1 calc R . . H7B H 0.4514 0.5893 0.4368 0.045 Uiso 1 1 calc R . . H7C H 0.5071 0.6530 0.3878 0.045 Uiso 1 1 calc R . . C8 C 0.2042(6) 0.5555(3) 0.4779(3) 0.0305(12) Uani 1 1 d . . . H8A H 0.1637 0.5205 0.4399 0.046 Uiso 1 1 calc R . . H8B H 0.1563 0.5508 0.5248 0.046 Uiso 1 1 calc R . . H8C H 0.3103 0.5479 0.4903 0.046 Uiso 1 1 calc R . . C9 C -0.0752(5) 0.6366(3) 0.5010(3) 0.0260(11) Uani 1 1 d . . . H9A H -0.1449 0.6089 0.4661 0.039 Uiso 1 1 calc R . . H9B H -0.1282 0.6742 0.5245 0.039 Uiso 1 1 calc R . . H9C H -0.0268 0.6059 0.5415 0.039 Uiso 1 1 calc R . . C10 C -0.1330(5) 0.7743(3) 0.4224(3) 0.0317(12) Uani 1 1 d . . . H10A H -0.2045 0.7612 0.3783 0.048 Uiso 1 1 calc R . . H10B H -0.1179 0.8254 0.4225 0.048 Uiso 1 1 calc R . . H10C H -0.1704 0.7602 0.4704 0.048 Uiso 1 1 calc R . . C11 C 0.0871(5) 0.8388(2) 0.3314(3) 0.0215(11) Uani 1 1 d . . . H11A H 0.0382 0.8295 0.2793 0.032 Uiso 1 1 calc R . . H11B H 0.1783 0.8650 0.3281 0.032 Uiso 1 1 calc R . . H11C H 0.0218 0.8667 0.3600 0.032 Uiso 1 1 calc R . . C12 C 0.3748(6) 0.7611(3) 0.3173(3) 0.0259(11) Uani 1 1 d . . . H12A H 0.3484 0.7463 0.2636 0.039 Uiso 1 1 calc R . . H12B H 0.4728 0.7430 0.3363 0.039 Uiso 1 1 calc R . . H12C H 0.3755 0.8126 0.3201 0.039 Uiso 1 1 calc R . . C13 C 0.2407(5) 0.8481(2) 0.5179(3) 0.0183(10) Uani 1 1 d . . . C21 C 0.2834(5) 0.9142(2) 0.4816(3) 0.0187(10) Uani 1 1 d . . . C22 C 0.3997(5) 0.9181(2) 0.4345(3) 0.0197(10) Uani 1 1 d . . . H22A H 0.4561 0.8771 0.4275 0.024 Uiso 1 1 calc R . . C23 C 0.4333(5) 0.9816(2) 0.3979(3) 0.0215(11) Uani 1 1 d . . . H23A H 0.5107 0.9831 0.3664 0.026 Uiso 1 1 calc R . . C24 C 0.3505(5) 1.0427(2) 0.4086(3) 0.0228(11) Uani 1 1 d . . . C25 C 0.2336(5) 1.0406(2) 0.4562(3) 0.0237(11) Uani 1 1 d . . . H25A H 0.1780 1.0818 0.4633 0.028 Uiso 1 1 calc R . . C26 C 0.2018(5) 0.9777(2) 0.4920(3) 0.0203(11) Uani 1 1 d . . . H26A H 0.1250 0.9767 0.5239 0.024 Uiso 1 1 calc R . . O3 O 0.3723(4) 1.10830(17) 0.3761(2) 0.0308(9) Uani 1 1 d . . . C33 C 0.4819(6) 1.1138(3) 0.3224(3) 0.0359(14) Uani 1 1 d . . . H33A H 0.4860 1.1625 0.3041 0.054 Uiso 1 1 calc R . . H33B H 0.4550 1.0824 0.2784 0.054 Uiso 1 1 calc R . . H33C H 0.5785 1.1002 0.3487 0.054 Uiso 1 1 calc R . . C14 C 0.1660(5) 0.8196(2) 0.5688(3) 0.0182(10) Uani 1 1 d . . . C27 C 0.0832(5) 0.8361(2) 0.6351(3) 0.0186(10) Uani 1 1 d . . . C28 C -0.0232(5) 0.7893(2) 0.6614(3) 0.0206(11) Uani 1 1 d . . . H28A H -0.0359 0.7436 0.6396 0.025 Uiso 1 1 calc R . . C29 C -0.1091(5) 0.8101(3) 0.7191(3) 0.0204(11) Uani 1 1 d . . . H29A H -0.1792 0.7785 0.7358 0.024 Uiso 1 1 calc R . . C30 C -0.0910(5) 0.8779(3) 0.7520(3) 0.0207(11) Uani 1 1 d . . . C31 C 0.0191(5) 0.9239(3) 0.7305(3) 0.0253(11) Uani 1 1 d . . . H31A H 0.0348 0.9684 0.7549 0.030 Uiso 1 1 calc R . . C32 C 0.1052(5) 0.9031(2) 0.6726(3) 0.0216(11) Uani 1 1 d . . . H32A H 0.1789 0.9339 0.6584 0.026 Uiso 1 1 calc R . . O4 O -0.1861(4) 0.89589(18) 0.80628(19) 0.0267(8) Uani 1 1 d . . . C34 C -0.1974(6) 0.9710(3) 0.8242(3) 0.0340(13) Uani 1 1 d . . . H34A H -0.2664 0.9773 0.8624 0.051 Uiso 1 1 calc R . . H34B H -0.2331 0.9969 0.7771 0.051 Uiso 1 1 calc R . . H34C H -0.1004 0.9890 0.8452 0.051 Uiso 1 1 calc R . . C15 C 0.4498(5) 0.7494(2) 0.5171(3) 0.0203(11) Uani 1 1 d . . . O1 O 0.5776(4) 0.75476(18) 0.5243(2) 0.0315(9) Uani 1 1 d . . . C16 C 0.2299(5) 0.6922(2) 0.5932(3) 0.0205(11) Uani 1 1 d . . . O2 O 0.2167(4) 0.66040(18) 0.6493(2) 0.0273(8) Uani 1 1 d . . . P P 0.35919(14) 0.39693(7) 0.30522(8) 0.0247(3) Uani 1 1 d . . . F1 F 0.2923(4) 0.47578(18) 0.2959(2) 0.0705(12) Uani 1 1 d . . . F2 F 0.2016(4) 0.3669(2) 0.3262(2) 0.0596(10) Uani 1 1 d . . . F3 F 0.3067(4) 0.38277(19) 0.21394(18) 0.0495(9) Uani 1 1 d . . . F4 F 0.4278(4) 0.31797(16) 0.3148(2) 0.0510(9) Uani 1 1 d . . . F5 F 0.4112(4) 0.41073(19) 0.3966(2) 0.0576(10) Uani 1 1 d . . . F6 F 0.5160(3) 0.4253(2) 0.2839(2) 0.0573(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 0.0172(4) 0.0154(4) 0.0154(4) 0.0001(3) 0.0026(3) 0.0006(3) C1 0.029(3) 0.018(2) 0.017(3) -0.006(2) 0.004(2) -0.001(2) C2 0.031(3) 0.017(2) 0.017(3) 0.001(2) 0.001(2) -0.002(2) C3 0.025(3) 0.020(3) 0.015(3) -0.005(2) 0.0031(19) -0.004(2) C4 0.019(2) 0.024(3) 0.017(3) -0.001(2) -0.0018(19) -0.002(2) C5 0.026(3) 0.018(2) 0.010(3) -0.0031(19) -0.0043(18) -0.004(2) C6 0.029(3) 0.017(2) 0.013(3) -0.0039(19) 0.0009(19) 0.000(2) C7 0.037(3) 0.023(3) 0.032(3) -0.002(2) 0.012(2) 0.005(2) C8 0.044(3) 0.018(3) 0.032(3) 0.006(2) 0.014(2) -0.001(2) C9 0.031(3) 0.024(3) 0.023(3) -0.004(2) 0.005(2) -0.008(2) C10 0.023(3) 0.039(3) 0.034(3) 0.006(2) 0.006(2) 0.006(2) C11 0.021(2) 0.024(3) 0.018(3) 0.003(2) -0.0017(19) -0.002(2) C12 0.037(3) 0.022(3) 0.021(3) 0.004(2) 0.012(2) -0.001(2) C13 0.016(2) 0.019(2) 0.019(3) -0.002(2) 0.001(2) -0.0013(19) C21 0.020(2) 0.019(2) 0.017(3) -0.003(2) -0.0015(19) -0.0020(19) C22 0.018(2) 0.019(2) 0.021(3) -0.005(2) -0.0023(19) 0.0026(19) C23 0.021(2) 0.021(3) 0.023(3) -0.003(2) 0.004(2) -0.005(2) C24 0.023(3) 0.020(3) 0.024(3) 0.005(2) -0.005(2) -0.005(2) C25 0.020(3) 0.019(3) 0.032(3) 0.000(2) 0.002(2) 0.0035(19) C26 0.017(2) 0.022(3) 0.021(3) -0.001(2) 0.0003(19) 0.0001(19) O3 0.030(2) 0.0219(19) 0.040(2) 0.0120(16) 0.0003(16) -0.0019(15) C33 0.029(3) 0.039(3) 0.040(4) 0.016(3) 0.003(2) -0.014(2) C14 0.014(2) 0.020(2) 0.019(3) -0.005(2) -0.0033(19) 0.0025(19) C27 0.019(2) 0.020(2) 0.016(3) -0.003(2) -0.0005(19) 0.0027(19) C28 0.023(2) 0.019(3) 0.020(3) -0.001(2) 0.000(2) 0.003(2) C29 0.012(2) 0.030(3) 0.019(3) 0.001(2) 0.0012(19) 0.0011(19) C30 0.016(2) 0.032(3) 0.014(3) 0.000(2) -0.0001(19) 0.008(2) C31 0.021(3) 0.022(3) 0.031(3) -0.007(2) -0.001(2) 0.004(2) C32 0.022(3) 0.026(3) 0.016(3) -0.003(2) -0.0026(19) -0.004(2) O4 0.0280(18) 0.032(2) 0.020(2) -0.0045(15) 0.0045(14) 0.0088(15) C34 0.033(3) 0.035(3) 0.034(3) -0.007(2) 0.006(2) 0.008(2) C15 0.026(3) 0.019(3) 0.016(3) 0.0036(19) 0.004(2) 0.004(2) O1 0.022(2) 0.038(2) 0.035(2) 0.0026(17) 0.0043(15) 0.0034(16) C16 0.018(2) 0.020(3) 0.023(3) -0.006(2) 0.000(2) 0.0037(19) O2 0.030(2) 0.031(2) 0.021(2) 0.0059(16) 0.0047(15) 0.0051(15) P 0.0248(7) 0.0220(7) 0.0270(8) -0.0036(6) 0.0012(5) -0.0027(5) F1 0.078(3) 0.037(2) 0.086(3) -0.0088(19) -0.032(2) 0.0264(19) F2 0.0342(19) 0.092(3) 0.057(2) -0.003(2) 0.0202(17) -0.0137(18) F3 0.050(2) 0.073(2) 0.0237(19) -0.0082(16) -0.0007(14) -0.0169(18) F4 0.065(2) 0.0260(17) 0.065(2) 0.0012(16) 0.0186(18) 0.0052(16) F5 0.070(2) 0.061(2) 0.037(2) -0.0164(17) -0.0140(17) 0.0078(19) F6 0.0333(19) 0.067(2) 0.068(3) 0.032(2) -0.0068(16) -0.0193(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C16 1.865(5) . ? Cr1 C15 1.895(5) . ? Cr1 C13 2.031(4) . ? Cr1 C14 2.059(4) . ? Cr1 C3 2.246(5) . ? Cr1 C6 2.276(5) . ? Cr1 C1 2.277(4) . ? Cr1 C2 2.283(5) . ? Cr1 C4 2.303(5) . ? Cr1 C5 2.310(5) . ? C1 C2 1.405(7) . ? C1 C6 1.434(6) . ? C1 C7 1.511(7) . ? C2 C3 1.436(7) . ? C2 C8 1.519(6) . ? C3 C4 1.419(7) . ? C3 C9 1.520(6) . ? C4 C5 1.415(6) . ? C4 C10 1.512(6) . ? C5 C6 1.430(6) . ? C5 C11 1.512(6) . ? C6 C12 1.513(6) . ? C13 C14 1.276(6) . ? C13 C21 1.450(6) . ? C21 C22 1.396(6) . ? C21 C26 1.412(6) . ? C22 C23 1.387(6) . ? C23 C24 1.381(6) . ? C24 O3 1.365(5) . ? C24 C25 1.405(7) . ? C25 C26 1.365(6) . ? O3 C33 1.428(6) . ? C14 C27 1.461(6) . ? C27 C32 1.405(6) . ? C27 C28 1.405(6) . ? C28 C29 1.378(6) . ? C29 C30 1.383(7) . ? C30 O4 1.376(5) . ? C30 C31 1.390(7) . ? C31 C32 1.383(7) . ? O4 C34 1.436(6) . ? C15 O1 1.142(5) . ? C16 O2 1.146(6) . ? P F1 1.585(3) . ? P F6 1.586(3) . ? P F4 1.592(3) . ? P F5 1.596(4) . ? P F3 1.597(3) . ? P F2 1.601(3) . ? 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 C16 Cr1 C15 92.21(19) . . ? C16 Cr1 C13 109.21(19) . . ? C15 Cr1 C13 83.80(18) . . ? C16 Cr1 C14 77.51(19) . . ? C15 Cr1 C14 102.43(18) . . ? C13 Cr1 C14 36.34(18) . . ? C16 Cr1 C3 83.91(18) . . ? C15 Cr1 C3 146.69(18) . . ? C13 Cr1 C3 128.72(17) . . ? C14 Cr1 C3 108.90(17) . . ? C16 Cr1 C6 147.12(18) . . ? C15 Cr1 C6 87.98(18) . . ? C13 Cr1 C6 103.50(17) . . ? C14 Cr1 C6 134.45(17) . . ? C3 Cr1 C6 78.23(16) . . ? C16 Cr1 C1 110.53(18) . . ? C15 Cr1 C1 84.87(18) . . ? C13 Cr1 C1 138.96(18) . . ? C14 Cr1 C1 169.16(18) . . ? C3 Cr1 C1 65.95(17) . . ? C6 Cr1 C1 36.72(16) . . ? C16 Cr1 C2 83.72(18) . . ? C15 Cr1 C2 109.77(18) . . ? C13 Cr1 C2 161.33(18) . . ? C14 Cr1 C2 143.16(17) . . ? C3 Cr1 C2 36.95(17) . . ? C6 Cr1 C2 65.46(16) . . ? C1 Cr1 C2 35.90(17) . . ? C16 Cr1 C4 113.10(18) . . ? C15 Cr1 C4 152.49(18) . . ? C13 Cr1 C4 97.05(17) . . ? C14 Cr1 C4 93.80(17) . . ? C3 Cr1 C4 36.32(17) . . ? C6 Cr1 C4 65.00(16) . . ? C1 Cr1 C4 76.49(17) . . ? C2 Cr1 C4 64.92(17) . . ? C16 Cr1 C5 148.39(18) . . ? C15 Cr1 C5 117.57(18) . . ? C13 Cr1 C5 85.78(17) . . ? C14 Cr1 C5 104.08(17) . . ? C3 Cr1 C5 65.50(16) . . ? C6 Cr1 C5 36.32(16) . . ? C1 Cr1 C5 65.21(16) . . ? C2 Cr1 C5 76.62(16) . . ? C4 Cr1 C5 35.73(16) . . ? C2 C1 C6 120.4(4) . . ? C2 C1 C7 119.4(4) . . ? C6 C1 C7 120.2(4) . . ? C2 C1 Cr1 72.3(3) . . ? C6 C1 Cr1 71.6(2) . . ? C7 C1 Cr1 130.0(3) . . ? C1 C2 C3 120.1(4) . . ? C1 C2 C8 118.7(4) . . ? C3 C2 C8 121.2(4) . . ? C1 C2 Cr1 71.8(3) . . ? C3 C2 Cr1 70.1(3) . . ? C8 C2 Cr1 130.2(3) . . ? C4 C3 C2 119.1(4) . . ? C4 C3 C9 120.2(4) . . ? C2 C3 C9 120.4(4) . . ? C4 C3 Cr1 74.0(3) . . ? C2 C3 Cr1 72.9(3) . . ? C9 C3 Cr1 129.0(3) . . ? C5 C4 C3 120.9(4) . . ? C5 C4 C10 120.5(4) . . ? C3 C4 C10 118.6(4) . . ? C5 C4 Cr1 72.4(3) . . ? C3 C4 Cr1 69.6(3) . . ? C10 C4 Cr1 130.4(3) . . ? C4 C5 C6 119.8(4) . . ? C4 C5 C11 119.1(4) . . ? C6 C5 C11 121.1(4) . . ? C4 C5 Cr1 71.9(3) . . ? C6 C5 Cr1 70.5(2) . . ? C11 C5 Cr1 132.9(3) . . ? C5 C6 C1 119.3(4) . . ? C5 C6 C12 121.2(4) . . ? C1 C6 C12 119.1(4) . . ? C5 C6 Cr1 73.1(3) . . ? C1 C6 Cr1 71.7(3) . . ? C12 C6 Cr1 132.8(3) . . ? C14 C13 C21 146.2(4) . . ? C14 C13 Cr1 73.1(3) . . ? C21 C13 Cr1 139.8(3) . . ? C22 C21 C26 117.7(4) . . ? C22 C21 C13 123.1(4) . . ? C26 C21 C13 119.2(4) . . ? C23 C22 C21 121.5(4) . . ? C24 C23 C22 119.4(4) . . ? O3 C24 C23 125.1(4) . . ? O3 C24 C25 114.6(4) . . ? C23 C24 C25 120.4(4) . . ? C26 C25 C24 119.7(4) . . ? C25 C26 C21 121.3(4) . . ? C24 O3 C33 118.0(4) . . ? C13 C14 C27 143.3(4) . . ? C13 C14 Cr1 70.6(3) . . ? C27 C14 Cr1 146.1(3) . . ? C32 C27 C28 117.7(4) . . ? C32 C27 C14 118.9(4) . . ? C28 C27 C14 123.3(4) . . ? C29 C28 C27 121.1(4) . . ? C28 C29 C30 119.9(4) . . ? O4 C30 C29 116.4(4) . . ? O4 C30 C31 123.2(4) . . ? C29 C30 C31 120.4(4) . . ? C32 C31 C30 119.6(4) . . ? C31 C32 C27 121.1(4) . . ? C30 O4 C34 116.5(4) . . ? O1 C15 Cr1 176.4(4) . . ? O2 C16 Cr1 175.6(4) . . ? F1 P F6 90.2(2) . . ? F1 P F4 179.5(2) . . ? F6 P F4 89.32(19) . . ? F1 P F5 90.7(2) . . ? F6 P F5 90.5(2) . . ? F4 P F5 89.1(2) . . ? F1 P F3 89.5(2) . . ? F6 P F3 89.68(19) . . ? F4 P F3 90.7(2) . . ? F5 P F3 179.7(2) . . ? F1 P F2 90.6(2) . . ? F6 P F2 179.0(2) . . ? F4 P F2 89.8(2) . . ? F5 P F2 89.8(2) . . ? F3 P F2 89.92(19) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.437 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.084 #===END data_4plus _database_code_CSD 189054 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H37 Cr F6 N O P' _chemical_formula_weight 696.64 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' 'F' 'F' 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.140(2) _cell_length_b 13.4946(15) _cell_length_c 22.153(3) _cell_angle_alpha 90 _cell_angle_beta 99.082(9) _cell_angle_gamma 90 _cell_volume 3288.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 185 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 0.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 17130 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5777 _reflns_number_gt 3967 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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. ; _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^)+(0.0553P)^2^+1.2604P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5777 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.77847(4) 0.10987(3) 0.22843(2) 0.02332(15) Uani 1 1 d . . . C1 C 0.6589(3) -0.0244(2) 0.19478(15) 0.0355(8) Uani 1 1 d . . . C2 C 0.7077(3) -0.0372(2) 0.25808(14) 0.0303(7) Uani 1 1 d . . . C3 C 0.8347(3) -0.0364(2) 0.27650(13) 0.0281(7) Uani 1 1 d . . . C4 C 0.9144(3) -0.0233(2) 0.23287(13) 0.0274(7) Uani 1 1 d . . . C5 C 0.8660(3) -0.0032(2) 0.17152(14) 0.0337(8) Uani 1 1 d . . . C6 C 0.7374(3) -0.0043(2) 0.15268(14) 0.0364(8) Uani 1 1 d . . . C7 C 0.5232(3) -0.0345(3) 0.17444(18) 0.0553(11) Uani 1 1 d . . . H7A H 0.5036 -0.1034 0.1630 0.083 Uiso 1 1 calc R . . H7B H 0.4978 0.0087 0.1391 0.083 Uiso 1 1 calc R . . H7C H 0.4804 -0.0151 0.2080 0.083 Uiso 1 1 calc R . . C8 C 0.6214(3) -0.0622(3) 0.30185(16) 0.0425(9) Uani 1 1 d . . . H8A H 0.6115 -0.1343 0.3035 0.064 Uiso 1 1 calc R . . H8B H 0.5423 -0.0313 0.2879 0.064 Uiso 1 1 calc R . . H8C H 0.6543 -0.0374 0.3427 0.064 Uiso 1 1 calc R . . C9 C 0.8885(3) -0.0514(3) 0.34295(14) 0.0407(9) Uani 1 1 d . . . H9A H 0.9037 -0.1221 0.3508 0.061 Uiso 1 1 calc R . . H9B H 0.8315 -0.0269 0.3690 0.061 Uiso 1 1 calc R . . H9C H 0.9652 -0.0148 0.3521 0.061 Uiso 1 1 calc R . . C10 C 1.0495(3) -0.0380(2) 0.25328(15) 0.0374(8) Uani 1 1 d . . . H10A H 1.0706 -0.1075 0.2473 0.056 Uiso 1 1 calc R . . H10B H 1.0705 -0.0208 0.2966 0.056 Uiso 1 1 calc R . . H10C H 1.0948 0.0047 0.2291 0.056 Uiso 1 1 calc R . . C11 C 0.9470(4) 0.0091(3) 0.12319(15) 0.0502(10) Uani 1 1 d . . . H11A H 0.9675 -0.0563 0.1084 0.075 Uiso 1 1 calc R . . H11B H 1.0217 0.0436 0.1408 0.075 Uiso 1 1 calc R . . H11C H 0.9041 0.0478 0.0890 0.075 Uiso 1 1 calc R . . C12 C 0.6848(4) 0.0119(3) 0.08571(14) 0.0569(11) Uani 1 1 d . . . H12A H 0.6776 -0.0519 0.0644 0.085 Uiso 1 1 calc R . . H12B H 0.7386 0.0557 0.0669 0.085 Uiso 1 1 calc R . . H12C H 0.6043 0.0425 0.0827 0.085 Uiso 1 1 calc R . . C13 C 0.9101(3) 0.1849(2) 0.28467(13) 0.0252(7) Uani 1 1 d . . . C21 C 1.0407(3) 0.2025(2) 0.29299(13) 0.0254(7) Uani 1 1 d . . . C22 C 1.1041(3) 0.2196(2) 0.35191(14) 0.0319(7) Uani 1 1 d . . . H22A H 1.0611 0.2233 0.3856 0.038 Uiso 1 1 calc R . . C23 C 1.2297(3) 0.2314(2) 0.36109(15) 0.0372(8) Uani 1 1 d . . . H23A H 1.2724 0.2431 0.4011 0.045 Uiso 1 1 calc R . . C24 C 1.2921(3) 0.2259(2) 0.31235(16) 0.0385(8) Uani 1 1 d . . . H24A H 1.3781 0.2327 0.3190 0.046 Uiso 1 1 calc R . . C25 C 1.2311(3) 0.2108(2) 0.25387(15) 0.0350(8) Uani 1 1 d . . . H25A H 1.2746 0.2082 0.2203 0.042 Uiso 1 1 calc R . . C26 C 1.1060(3) 0.1993(2) 0.24455(13) 0.0281(7) Uani 1 1 d . . . H26A H 1.0641 0.1891 0.2043 0.034 Uiso 1 1 calc R . . C14 C 0.8131(3) 0.1944(2) 0.30816(12) 0.0260(7) Uani 1 1 d . . . C27 C 0.7535(3) 0.2356(2) 0.35679(13) 0.0258(7) Uani 1 1 d . . . C28 C 0.7843(3) 0.3303(2) 0.37925(14) 0.0366(8) Uani 1 1 d . . . H28A H 0.8442 0.3674 0.3629 0.044 Uiso 1 1 calc R . . C29 C 0.7287(3) 0.3708(3) 0.42514(15) 0.0449(9) Uani 1 1 d . . . H29A H 0.7502 0.4356 0.4398 0.054 Uiso 1 1 calc R . . C30 C 0.6424(3) 0.3176(3) 0.44977(14) 0.0416(9) Uani 1 1 d . . . H30A H 0.6047 0.3455 0.4814 0.050 Uiso 1 1 calc R . . C31 C 0.6112(3) 0.2239(3) 0.42833(14) 0.0418(9) Uani 1 1 d . . . H31A H 0.5527 0.1866 0.4456 0.050 Uiso 1 1 calc R . . C32 C 0.6651(3) 0.1837(2) 0.38150(14) 0.0353(8) Uani 1 1 d . . . H32A H 0.6411 0.1198 0.3661 0.042 Uiso 1 1 calc R . . C15 C 0.6308(3) 0.1660(2) 0.23686(13) 0.0282(7) Uani 1 1 d . . . O1 O 0.5387(2) 0.19911(18) 0.24413(10) 0.0422(6) Uani 1 1 d . . . C16 C 0.7961(3) 0.2086(2) 0.16561(13) 0.0266(7) Uani 1 1 d . . . N1 N 0.8046(2) 0.26745(19) 0.12763(11) 0.0303(6) Uani 1 1 d . . . C33 C 0.8025(3) 0.3450(2) 0.08541(13) 0.0303(7) Uani 1 1 d . . . C34 C 0.8801(3) 0.3404(2) 0.04169(13) 0.0324(8) Uani 1 1 d . . . C35 C 0.8770(3) 0.4194(3) 0.00169(15) 0.0438(9) Uani 1 1 d . . . H35A H 0.9286 0.4189 -0.0286 0.053 Uiso 1 1 calc R . . C36 C 0.8006(4) 0.4983(3) 0.00488(17) 0.0525(10) Uani 1 1 d . . . H36A H 0.8006 0.5521 -0.0228 0.063 Uiso 1 1 calc R . . C37 C 0.7240(4) 0.5001(3) 0.04807(17) 0.0516(10) Uani 1 1 d . . . H37A H 0.6709 0.5550 0.0494 0.062 Uiso 1 1 calc R . . C38 C 0.7230(3) 0.4234(2) 0.08958(15) 0.0377(8) Uani 1 1 d . . . C39 C 0.6402(4) 0.4244(3) 0.13692(18) 0.0553(11) Uani 1 1 d . . . H39A H 0.5914 0.4852 0.1327 0.083 Uiso 1 1 calc R . . H39B H 0.6889 0.4221 0.1778 0.083 Uiso 1 1 calc R . . H39C H 0.5862 0.3667 0.1312 0.083 Uiso 1 1 calc R . . C40 C 0.9628(3) 0.2534(3) 0.03789(16) 0.0464(9) Uani 1 1 d . . . H40A H 1.0097 0.2639 0.0046 0.070 Uiso 1 1 calc R . . H40B H 0.9141 0.1929 0.0301 0.070 Uiso 1 1 calc R . . H40C H 1.0185 0.2466 0.0766 0.070 Uiso 1 1 calc R . . P1 P 0.33060(9) 0.19640(7) 0.06102(4) 0.0393(2) Uani 1 1 d . . . F1 F 0.3932(3) 0.2626(2) 0.01687(13) 0.1010(10) Uani 1 1 d . . . F2 F 0.3987(2) 0.10159(18) 0.04088(10) 0.0743(8) Uani 1 1 d . . . F3 F 0.2666(3) 0.12833(19) 0.10489(13) 0.0998(10) Uani 1 1 d . . . F4 F 0.2606(2) 0.28885(17) 0.08250(11) 0.0791(8) Uani 1 1 d . . . F5 F 0.2217(2) 0.1770(2) 0.00716(10) 0.0798(8) Uani 1 1 d . . . F6 F 0.4393(2) 0.21504(18) 0.11457(10) 0.0807(8) 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 0.0266(3) 0.0208(3) 0.0224(2) 0.0003(2) 0.00317(19) 0.0032(2) C1 0.034(2) 0.0215(17) 0.048(2) -0.0054(15) -0.0053(16) 0.0039(14) C2 0.035(2) 0.0181(16) 0.0367(18) -0.0019(13) 0.0031(15) -0.0024(13) C3 0.034(2) 0.0170(15) 0.0315(16) 0.0011(13) 0.0007(14) 0.0017(13) C4 0.0315(19) 0.0177(16) 0.0322(17) 0.0002(13) 0.0021(14) 0.0052(13) C5 0.046(2) 0.0251(17) 0.0303(17) -0.0021(14) 0.0055(15) 0.0115(15) C6 0.053(2) 0.0231(17) 0.0290(17) -0.0066(14) -0.0055(16) 0.0115(16) C7 0.040(2) 0.047(2) 0.070(3) -0.004(2) -0.0181(19) -0.0008(18) C8 0.037(2) 0.032(2) 0.060(2) 0.0031(17) 0.0131(17) -0.0053(16) C9 0.046(2) 0.042(2) 0.0328(18) 0.0097(16) 0.0016(16) -0.0009(17) C10 0.033(2) 0.0293(19) 0.050(2) 0.0033(16) 0.0071(16) 0.0084(15) C11 0.068(3) 0.048(2) 0.040(2) 0.0009(18) 0.0245(19) 0.026(2) C12 0.080(3) 0.057(3) 0.0275(18) -0.0093(18) -0.0120(19) 0.017(2) C13 0.0303(18) 0.0198(16) 0.0258(16) 0.0016(13) 0.0055(14) -0.0008(13) C21 0.0281(18) 0.0179(16) 0.0307(16) 0.0012(13) 0.0060(13) 0.0006(13) C22 0.035(2) 0.0319(18) 0.0294(17) -0.0034(14) 0.0074(14) -0.0006(14) C23 0.034(2) 0.039(2) 0.0365(19) -0.0038(16) -0.0014(15) -0.0036(15) C24 0.028(2) 0.034(2) 0.052(2) 0.0002(17) 0.0041(16) -0.0017(15) C25 0.034(2) 0.0316(19) 0.043(2) 0.0009(15) 0.0151(16) 0.0012(15) C26 0.0305(19) 0.0251(17) 0.0288(16) 0.0002(13) 0.0048(14) -0.0006(14) C14 0.0332(19) 0.0215(16) 0.0228(15) 0.0027(13) 0.0029(14) -0.0006(13) C27 0.0250(17) 0.0271(17) 0.0245(16) -0.0020(13) 0.0010(13) 0.0059(13) C28 0.038(2) 0.037(2) 0.0351(18) -0.0061(16) 0.0060(15) -0.0058(16) C29 0.052(2) 0.042(2) 0.038(2) -0.0160(17) -0.0015(17) 0.0096(18) C30 0.038(2) 0.061(3) 0.0252(17) -0.0075(17) 0.0042(15) 0.0133(18) C31 0.036(2) 0.060(3) 0.0316(18) -0.0023(18) 0.0109(15) 0.0027(17) C32 0.039(2) 0.0349(19) 0.0333(18) -0.0036(15) 0.0110(15) -0.0047(15) C15 0.030(2) 0.0287(18) 0.0251(16) 0.0026(14) 0.0010(14) -0.0026(15) O1 0.0298(15) 0.0550(16) 0.0418(13) -0.0042(12) 0.0054(11) 0.0100(12) C16 0.0253(18) 0.0286(18) 0.0257(16) -0.0046(14) 0.0035(13) 0.0050(13) N1 0.0345(16) 0.0322(15) 0.0242(14) 0.0015(13) 0.0044(12) -0.0006(12) C33 0.0344(19) 0.0298(18) 0.0261(16) 0.0050(14) 0.0025(14) -0.0073(15) C34 0.0289(19) 0.041(2) 0.0258(16) -0.0032(15) 0.0003(14) -0.0103(15) C35 0.055(2) 0.050(2) 0.0282(18) 0.0041(17) 0.0118(16) -0.0200(19) C36 0.072(3) 0.041(2) 0.044(2) 0.0150(18) 0.008(2) -0.014(2) C37 0.063(3) 0.034(2) 0.059(2) 0.0118(19) 0.010(2) 0.0076(19) C38 0.038(2) 0.0295(19) 0.047(2) 0.0035(16) 0.0113(16) -0.0013(15) C39 0.055(3) 0.047(2) 0.070(3) 0.000(2) 0.029(2) 0.0081(19) C40 0.040(2) 0.058(3) 0.044(2) -0.0063(18) 0.0131(17) -0.0010(18) P1 0.0494(6) 0.0379(5) 0.0298(5) -0.0044(4) 0.0037(4) 0.0092(4) F1 0.091(2) 0.124(3) 0.093(2) 0.0542(18) 0.0335(16) 0.0023(18) F2 0.0761(17) 0.0739(17) 0.0657(15) -0.0267(13) -0.0113(12) 0.0346(13) F3 0.150(3) 0.0689(19) 0.095(2) 0.0051(15) 0.0616(19) -0.0190(18) F4 0.090(2) 0.0570(15) 0.0895(18) -0.0301(13) 0.0111(15) 0.0246(13) F5 0.0497(15) 0.118(2) 0.0655(15) -0.0361(15) -0.0104(12) 0.0251(14) F6 0.095(2) 0.0709(17) 0.0616(15) -0.0178(13) -0.0329(14) 0.0093(14) _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 C15 1.847(3) . ? Cr1 C16 1.959(3) . ? Cr1 C13 2.037(3) . ? Cr1 C14 2.087(3) . ? Cr1 C2 2.270(3) . ? Cr1 C6 2.271(3) . ? Cr1 C3 2.283(3) . ? Cr1 C5 2.293(3) . ? Cr1 C1 2.302(3) . ? Cr1 C4 2.342(3) . ? C1 C6 1.401(5) . ? C1 C2 1.432(4) . ? C1 C7 1.514(5) . ? C2 C3 1.410(4) . ? C2 C8 1.507(4) . ? C3 C4 1.423(4) . ? C3 C9 1.513(4) . ? C4 C5 1.407(4) . ? C4 C10 1.514(4) . ? C5 C6 1.428(5) . ? C5 C11 1.514(4) . ? C6 C12 1.523(4) . ? C13 C14 1.277(4) . ? C13 C21 1.458(4) . ? C21 C26 1.389(4) . ? C21 C22 1.401(4) . ? C22 C23 1.391(4) . ? C23 C24 1.376(4) . ? C24 C25 1.380(5) . ? C25 C26 1.385(4) . ? C14 C27 1.462(4) . ? C27 C32 1.389(4) . ? C27 C28 1.395(4) . ? C28 C29 1.384(4) . ? C29 C30 1.380(5) . ? C30 C31 1.376(5) . ? C31 C32 1.388(4) . ? C15 O1 1.154(3) . ? C16 N1 1.171(4) . ? N1 C33 1.402(4) . ? C33 C38 1.391(5) . ? C33 C34 1.398(4) . ? C34 C35 1.383(4) . ? C34 C40 1.503(5) . ? C35 C36 1.372(5) . ? C36 C37 1.380(5) . ? C37 C38 1.387(5) . ? C38 C39 1.502(5) . ? P1 F1 1.567(3) . ? P1 F6 1.576(2) . ? P1 F4 1.584(2) . ? P1 F5 1.584(2) . ? P1 F3 1.586(3) . ? P1 F2 1.587(2) . ? 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 C15 Cr1 C16 89.06(12) . . ? C15 Cr1 C13 107.51(13) . . ? C16 Cr1 C13 87.32(12) . . ? C15 Cr1 C14 74.87(12) . . ? C16 Cr1 C14 101.74(12) . . ? C13 Cr1 C14 36.06(11) . . ? C15 Cr1 C2 88.47(12) . . ? C16 Cr1 C2 151.46(12) . . ? C13 Cr1 C2 120.45(11) . . ? C14 Cr1 C2 105.01(11) . . ? C15 Cr1 C6 105.91(13) . . ? C16 Cr1 C6 88.16(12) . . ? C13 Cr1 C6 146.18(13) . . ? C14 Cr1 C6 170.10(11) . . ? C2 Cr1 C6 65.30(11) . . ? C15 Cr1 C3 119.38(12) . . ? C16 Cr1 C3 150.31(12) . . ? C13 Cr1 C3 91.50(11) . . ? C14 Cr1 C3 94.43(11) . . ? C2 Cr1 C3 36.08(10) . . ? C6 Cr1 C3 76.50(11) . . ? C15 Cr1 C5 142.32(13) . . ? C16 Cr1 C5 87.90(11) . . ? C13 Cr1 C5 109.84(12) . . ? C14 Cr1 C5 142.30(12) . . ? C2 Cr1 C5 76.98(11) . . ? C6 Cr1 C5 36.47(12) . . ? C3 Cr1 C5 64.64(11) . . ? C15 Cr1 C1 82.91(12) . . ? C16 Cr1 C1 115.04(12) . . ? C13 Cr1 C1 155.91(11) . . ? C14 Cr1 C1 136.44(12) . . ? C2 Cr1 C1 36.49(11) . . ? C6 Cr1 C1 35.68(12) . . ? C3 Cr1 C1 64.70(11) . . ? C5 Cr1 C1 64.69(12) . . ? C15 Cr1 C4 152.95(12) . . ? C16 Cr1 C4 114.54(11) . . ? C13 Cr1 C4 87.56(11) . . ? C14 Cr1 C4 110.60(11) . . ? C2 Cr1 C4 64.48(11) . . ? C6 Cr1 C4 64.16(11) . . ? C3 Cr1 C4 35.80(10) . . ? C5 Cr1 C4 35.32(10) . . ? C1 Cr1 C4 75.33(11) . . ? C6 C1 C2 119.7(3) . . ? C6 C1 C7 121.2(3) . . ? C2 C1 C7 119.1(3) . . ? C6 C1 Cr1 70.94(18) . . ? C2 C1 Cr1 70.55(17) . . ? C7 C1 Cr1 131.8(2) . . ? C3 C2 C1 119.4(3) . . ? C3 C2 C8 121.9(3) . . ? C1 C2 C8 118.4(3) . . ? C3 C2 Cr1 72.45(17) . . ? C1 C2 Cr1 72.96(18) . . ? C8 C2 Cr1 131.9(2) . . ? C2 C3 C4 120.7(3) . . ? C2 C3 C9 120.4(3) . . ? C4 C3 C9 119.0(3) . . ? C2 C3 Cr1 71.47(17) . . ? C4 C3 Cr1 74.36(17) . . ? C9 C3 Cr1 127.4(2) . . ? C5 C4 C3 119.7(3) . . ? C5 C4 C10 121.7(3) . . ? C3 C4 C10 118.6(3) . . ? C5 C4 Cr1 70.43(17) . . ? C3 C4 Cr1 69.84(16) . . ? C10 C4 Cr1 135.9(2) . . ? C4 C5 C6 119.6(3) . . ? C4 C5 C11 121.6(3) . . ? C6 C5 C11 118.5(3) . . ? C4 C5 Cr1 74.24(17) . . ? C6 C5 Cr1 70.91(17) . . ? C11 C5 Cr1 131.9(2) . . ? C1 C6 C5 120.7(3) . . ? C1 C6 C12 119.5(3) . . ? C5 C6 C12 119.8(3) . . ? C1 C6 Cr1 73.37(18) . . ? C5 C6 Cr1 72.62(17) . . ? C12 C6 Cr1 128.6(2) . . ? C14 C13 C21 145.5(3) . . ? C14 C13 Cr1 74.09(19) . . ? C21 C13 Cr1 140.0(2) . . ? C26 C21 C22 118.5(3) . . ? C26 C21 C13 122.1(3) . . ? C22 C21 C13 119.4(3) . . ? C23 C22 C21 120.1(3) . . ? C24 C23 C22 120.1(3) . . ? C23 C24 C25 120.7(3) . . ? C24 C25 C26 119.4(3) . . ? C25 C26 C21 121.2(3) . . ? C13 C14 C27 148.3(3) . . ? C13 C14 Cr1 69.85(18) . . ? C27 C14 Cr1 141.9(2) . . ? C32 C27 C28 118.1(3) . . ? C32 C27 C14 122.1(3) . . ? C28 C27 C14 119.7(3) . . ? C29 C28 C27 120.7(3) . . ? C30 C29 C28 120.4(3) . . ? C31 C30 C29 119.7(3) . . ? C30 C31 C32 120.1(3) . . ? C31 C32 C27 121.0(3) . . ? O1 C15 Cr1 177.5(3) . . ? N1 C16 Cr1 178.9(3) . . ? C16 N1 C33 172.2(3) . . ? C38 C33 C34 123.3(3) . . ? C38 C33 N1 117.8(3) . . ? C34 C33 N1 118.9(3) . . ? C35 C34 C33 117.0(3) . . ? C35 C34 C40 121.3(3) . . ? C33 C34 C40 121.7(3) . . ? C36 C35 C34 121.2(3) . . ? C35 C36 C37 120.4(3) . . ? C36 C37 C38 121.1(3) . . ? C37 C38 C33 116.9(3) . . ? C37 C38 C39 121.7(3) . . ? C33 C38 C39 121.4(3) . . ? F1 P1 F6 90.82(16) . . ? F1 P1 F4 91.58(16) . . ? F6 P1 F4 90.23(14) . . ? F1 P1 F5 89.30(16) . . ? F6 P1 F5 179.64(15) . . ? F4 P1 F5 90.11(14) . . ? F1 P1 F3 179.14(18) . . ? F6 P1 F3 89.86(16) . . ? F4 P1 F3 88.95(15) . . ? F5 P1 F3 90.02(17) . . ? F1 P1 F2 90.23(16) . . ? F6 P1 F2 89.77(13) . . ? F4 P1 F2 178.19(16) . . ? F5 P1 F2 89.90(12) . . ? F3 P1 F2 89.24(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.396 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.057 #===END data_6plus _database_code_CSD 189055 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H37 Cr F6 O4 P2' _chemical_formula_weight 689.54 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.993(4) _cell_length_b 26.514(6) _cell_length_c 28.425(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 12807(5) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 254 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5712 _exptl_absorpt_coefficient_mu 0.526 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7047 _exptl_absorpt_correction_T_max 0.7713 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _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 with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 62123 _diffrn_reflns_av_R_equivalents 0.2230 _diffrn_reflns_av_sigmaI/netI 0.1821 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 24.00 _reflns_number_total 10056 _reflns_number_gt 4212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. ; _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^)+(0.0650P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10056 _refine_ls_number_parameters 775 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1836 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1600 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.901 _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 1.05272(6) -0.20376(4) 0.53963(4) 0.0296(3) Uani 1 1 d . . . C1 C 1.0120(6) -0.1267(2) 0.5694(3) 0.056(3) Uani 1 1 d . . . C2 C 1.0937(6) -0.1238(3) 0.5607(3) 0.049(2) Uani 1 1 d . . . C3 C 1.1247(4) -0.1361(3) 0.5166(3) 0.040(2) Uani 1 1 d . . . C4 C 1.0728(5) -0.1488(3) 0.4793(3) 0.041(2) Uani 1 1 d . . . C5 C 0.9918(5) -0.1511(2) 0.4869(3) 0.042(2) Uani 1 1 d . . . C6 C 0.9615(4) -0.1404(3) 0.5316(3) 0.048(2) Uani 1 1 d . . . C7 C 0.9804(6) -0.1125(3) 0.6166(3) 0.092(4) Uani 1 1 d . . . H7A H 0.9689 -0.0763 0.6172 0.138 Uiso 1 1 calc R . . H7B H 1.0196 -0.1204 0.6409 0.138 Uiso 1 1 calc R . . H7C H 0.9320 -0.1315 0.6229 0.138 Uiso 1 1 calc R . . C8 C 1.1498(6) -0.1024(3) 0.5976(3) 0.107(4) Uani 1 1 d . . . H8A H 1.1511 -0.0656 0.5950 0.160 Uiso 1 1 calc R . . H8B H 1.2028 -0.1159 0.5923 0.160 Uiso 1 1 calc R . . H8C H 1.1316 -0.1120 0.6291 0.160 Uiso 1 1 calc R . . C9 C 1.2116(4) -0.1328(3) 0.5074(3) 0.085(3) Uani 1 1 d . . . H9A H 1.2252 -0.0984 0.4979 0.127 Uiso 1 1 calc R . . H9B H 1.2259 -0.1564 0.4822 0.127 Uiso 1 1 calc R . . H9C H 1.2405 -0.1416 0.5361 0.127 Uiso 1 1 calc R . . C10 C 1.1044(5) -0.1561(3) 0.4301(3) 0.072(3) Uani 1 1 d . . . H10A H 1.1049 -0.1236 0.4136 0.108 Uiso 1 1 calc R . . H10B H 1.0707 -0.1798 0.4130 0.108 Uiso 1 1 calc R . . H10C H 1.1581 -0.1695 0.4317 0.108 Uiso 1 1 calc R . . C11 C 0.9360(5) -0.1639(3) 0.4468(3) 0.079(3) Uani 1 1 d . . . H11A H 0.9201 -0.1328 0.4307 0.118 Uiso 1 1 calc R . . H11B H 0.8893 -0.1808 0.4595 0.118 Uiso 1 1 calc R . . H11C H 0.9626 -0.1862 0.4245 0.118 Uiso 1 1 calc R . . C12 C 0.8718(5) -0.1393(3) 0.5386(4) 0.092(4) Uani 1 1 d . . . H12A H 0.8519 -0.1053 0.5320 0.138 Uiso 1 1 calc R . . H12B H 0.8592 -0.1484 0.5712 0.138 Uiso 1 1 calc R . . H12C H 0.8469 -0.1634 0.5172 0.138 Uiso 1 1 calc R . . C13 C 0.9613(4) -0.2435(2) 0.5666(2) 0.0271(17) Uani 1 1 d . . . C14 C 0.9817(3) -0.2661(2) 0.5292(3) 0.0291(17) Uani 1 1 d . . . C15 C 1.1140(4) -0.2448(3) 0.5030(3) 0.0339(19) Uani 1 1 d . . . O1 O 1.1544(3) -0.26925(18) 0.47923(18) 0.0484(14) Uani 1 1 d . . . C21 C 0.9002(4) -0.2429(2) 0.6029(3) 0.0295(18) Uani 1 1 d . . . C22 C 0.8215(4) -0.2528(2) 0.5903(3) 0.0374(19) Uani 1 1 d . . . H22A H 0.8090 -0.2611 0.5587 0.045 Uiso 1 1 calc R . . C23 C 0.7621(4) -0.2506(2) 0.6238(3) 0.042(2) Uani 1 1 d . . . H23A H 0.7090 -0.2569 0.6150 0.050 Uiso 1 1 calc R . . C24 C 0.7802(4) -0.2394(2) 0.6698(3) 0.0391(19) Uani 1 1 d . . . H24A H 0.7395 -0.2385 0.6927 0.047 Uiso 1 1 calc R . . C25 C 0.8563(4) -0.2295(2) 0.6830(3) 0.0386(19) Uani 1 1 d . . . H25A H 0.8680 -0.2217 0.7148 0.046 Uiso 1 1 calc R . . C26 C 0.9168(4) -0.2309(2) 0.6497(3) 0.0340(18) Uani 1 1 d . . . H26A H 0.9693 -0.2236 0.6589 0.041 Uiso 1 1 calc R . . C27 C 0.9653(3) -0.3078(2) 0.4974(2) 0.0272(17) Uani 1 1 d . . . C28 C 0.9839(4) -0.3072(3) 0.4498(2) 0.0329(18) Uani 1 1 d . . . H28A H 1.0108 -0.2790 0.4369 0.039 Uiso 1 1 calc R . . C29 C 0.9635(4) -0.3473(3) 0.4207(2) 0.0358(18) Uani 1 1 d . . . H29A H 0.9767 -0.3463 0.3882 0.043 Uiso 1 1 calc R . . C30 C 0.9247(4) -0.3884(3) 0.4385(3) 0.0340(19) Uani 1 1 d . . . H30A H 0.9103 -0.4154 0.4184 0.041 Uiso 1 1 calc R . . C31 C 0.9067(4) -0.3903(3) 0.4857(3) 0.0372(19) Uani 1 1 d . . . H31A H 0.8807 -0.4191 0.4981 0.045 Uiso 1 1 calc R . . C32 C 0.9259(4) -0.3507(2) 0.5150(2) 0.0327(18) Uani 1 1 d . . . H32A H 0.9126 -0.3523 0.5475 0.039 Uiso 1 1 calc R . . P1 P 1.12666(11) -0.23223(7) 0.60189(7) 0.0367(5) Uani 1 1 d . . . O2 O 1.1135(3) -0.20338(17) 0.64988(16) 0.0440(13) Uani 1 1 d . . . C33 C 1.1430(5) -0.2173(3) 0.6951(3) 0.082(3) Uani 1 1 d . . . H33A H 1.1259 -0.1925 0.7185 0.124 Uiso 1 1 calc R . . H33B H 1.2006 -0.2183 0.6941 0.124 Uiso 1 1 calc R . . H33C H 1.1228 -0.2507 0.7036 0.124 Uiso 1 1 calc R . . O3 O 1.1147(3) -0.28884(18) 0.62052(19) 0.0557(15) Uani 1 1 d . . . C34 C 1.1273(5) -0.3316(3) 0.5911(3) 0.082(3) Uani 1 1 d . . . H34A H 1.1169 -0.3625 0.6090 0.123 Uiso 1 1 calc R . . H34B H 1.1819 -0.3317 0.5801 0.123 Uiso 1 1 calc R . . H34C H 1.0917 -0.3300 0.5640 0.123 Uiso 1 1 calc R . . O4 O 1.2170(3) -0.22678(19) 0.58934(18) 0.0534(15) Uani 1 1 d . . . C35 C 1.2833(5) -0.2427(4) 0.6162(4) 0.090(3) Uani 1 1 d . . . H35A H 1.3317 -0.2341 0.5994 0.135 Uiso 1 1 calc R . . H35B H 1.2808 -0.2793 0.6210 0.135 Uiso 1 1 calc R . . H35C H 1.2828 -0.2257 0.6468 0.135 Uiso 1 1 calc R . . P2 P 1.24795(12) -0.04336(8) 0.07451(8) 0.0439(5) Uani 1 1 d . . . F1 F 1.2997(3) -0.0384(2) 0.0299(2) 0.126(2) Uani 1 1 d . . . F2 F 1.2076(3) 0.00903(16) 0.0641(2) 0.0911(18) Uani 1 1 d . . . F3 F 1.2876(2) -0.09646(16) 0.08706(17) 0.0704(14) Uani 1 1 d . . . F4 F 1.3141(2) -0.01574(17) 0.1049(2) 0.0866(18) Uani 1 1 d . . . F5 F 1.1811(3) -0.07094(17) 0.04635(16) 0.0777(15) Uani 1 1 d . . . F6 F 1.1967(2) -0.04978(18) 0.12112(16) 0.0720(14) Uani 1 1 d . . . Cr2 Cr 0.83766(6) 0.00278(4) 0.15804(4) 0.0315(3) Uani 1 1 d . . . C101 C 0.9107(4) 0.0392(3) 0.1002(3) 0.047(2) Uani 1 1 d . . . C102 C 0.9605(4) 0.0062(3) 0.1273(3) 0.0381(19) Uani 1 1 d . . . C103 C 0.9707(4) 0.0133(3) 0.1748(3) 0.039(2) Uani 1 1 d . . . C104 C 0.9258(4) 0.0514(3) 0.1990(3) 0.044(2) Uani 1 1 d . . . C105 C 0.8774(4) 0.0843(3) 0.1712(4) 0.049(2) Uani 1 1 d . . . C106 C 0.8716(4) 0.0783(3) 0.1230(3) 0.046(2) Uani 1 1 d . . . C107 C 0.9051(5) 0.0336(3) 0.0475(3) 0.070(3) Uani 1 1 d . . . H10D H 0.9454 0.0546 0.0325 0.105 Uiso 1 1 calc R . . H10E H 0.8529 0.0444 0.0369 0.105 Uiso 1 1 calc R . . H10F H 0.9135 -0.0018 0.0389 0.105 Uiso 1 1 calc R . . C108 C 1.0057(4) -0.0352(3) 0.1010(3) 0.062(3) Uani 1 1 d . . . H10G H 1.0577 -0.0225 0.0920 0.093 Uiso 1 1 calc R . . H10H H 0.9764 -0.0449 0.0727 0.093 Uiso 1 1 calc R . . H10I H 1.0118 -0.0646 0.1215 0.093 Uiso 1 1 calc R . . C109 C 1.0314(4) -0.0170(3) 0.2020(3) 0.060(3) Uani 1 1 d . . . H10J H 1.0822 0.0004 0.2009 0.091 Uiso 1 1 calc R . . H10K H 1.0367 -0.0505 0.1878 0.091 Uiso 1 1 calc R . . H10L H 1.0144 -0.0205 0.2348 0.091 Uiso 1 1 calc R . . C110 C 0.9362(5) 0.0585(3) 0.2514(3) 0.080(3) Uani 1 1 d . . . H11D H 0.9795 0.0821 0.2573 0.120 Uiso 1 1 calc R . . H11E H 0.9482 0.0259 0.2661 0.120 Uiso 1 1 calc R . . H11F H 0.8875 0.0721 0.2649 0.120 Uiso 1 1 calc R . . C111 C 0.8397(5) 0.1293(3) 0.1955(4) 0.090(4) Uani 1 1 d . . . H11G H 0.8754 0.1583 0.1940 0.135 Uiso 1 1 calc R . . H11H H 0.8292 0.1209 0.2285 0.135 Uiso 1 1 calc R . . H11I H 0.7901 0.1378 0.1798 0.135 Uiso 1 1 calc R . . C112 C 0.8203(5) 0.1152(3) 0.0950(4) 0.090(4) Uani 1 1 d . . . H11J H 0.8524 0.1439 0.0848 0.135 Uiso 1 1 calc R . . H11K H 0.7772 0.1272 0.1150 0.135 Uiso 1 1 calc R . . H11L H 0.7986 0.0980 0.0674 0.135 Uiso 1 1 calc R . . C113 C 0.7374(4) 0.0236(2) 0.1911(2) 0.0277(17) Uani 1 1 d . . . C114 C 0.7173(4) 0.0064(2) 0.1513(2) 0.0294(17) Uani 1 1 d . . . C115 C 0.8143(4) -0.0417(3) 0.1113(3) 0.0345(19) Uani 1 1 d . . . O101 O 0.8009(3) -0.06994(19) 0.08080(18) 0.0463(14) Uani 1 1 d . . . C121 C 0.7083(4) 0.0510(2) 0.2331(3) 0.0310(18) Uani 1 1 d . . . C122 C 0.7320(4) 0.0386(3) 0.2781(3) 0.0383(19) Uani 1 1 d . . . H12D H 0.7681 0.0117 0.2828 0.046 Uiso 1 1 calc R . . C123 C 0.7035(4) 0.0653(3) 0.3166(3) 0.047(2) Uani 1 1 d . . . H12E H 0.7189 0.0558 0.3475 0.057 Uiso 1 1 calc R . . C124 C 0.6523(4) 0.1058(3) 0.3102(3) 0.049(2) Uani 1 1 d . . . H12F H 0.6341 0.1248 0.3364 0.059 Uiso 1 1 calc R . . C125 C 0.6288(4) 0.1178(3) 0.2652(3) 0.042(2) Uani 1 1 d . . . H12G H 0.5939 0.1453 0.2605 0.051 Uiso 1 1 calc R . . C126 C 0.6546(4) 0.0907(3) 0.2271(3) 0.0388(19) Uani 1 1 d . . . H12H H 0.6361 0.0989 0.1965 0.047 Uiso 1 1 calc R . . C127 C 0.6482(3) -0.0056(2) 0.1226(2) 0.0271(16) Uani 1 1 d . . . C128 C 0.5792(4) -0.0197(2) 0.1460(3) 0.0381(19) Uani 1 1 d . . . H12I H 0.5785 -0.0222 0.1793 0.046 Uiso 1 1 calc R . . C129 C 0.5122(4) -0.0300(3) 0.1203(3) 0.048(2) Uani 1 1 d . . . H12J H 0.4652 -0.0392 0.1363 0.058 Uiso 1 1 calc R . . C130 C 0.5124(4) -0.0273(3) 0.0716(3) 0.049(2) Uani 1 1 d . . . H13A H 0.4660 -0.0342 0.0541 0.058 Uiso 1 1 calc R . . C131 C 0.5816(5) -0.0141(3) 0.0490(3) 0.048(2) Uani 1 1 d . . . H13B H 0.5824 -0.0126 0.0156 0.057 Uiso 1 1 calc R . . C132 C 0.6496(4) -0.0032(3) 0.0737(2) 0.0337(17) Uani 1 1 d . . . H13C H 0.6965 0.0058 0.0576 0.040 Uiso 1 1 calc R . . P101 P 0.83994(11) -0.06671(7) 0.20582(7) 0.0388(5) Uani 1 1 d . . . O102 O 0.8643(3) -0.05891(17) 0.25859(17) 0.0524(14) Uani 1 1 d . . . C133 C 0.8505(5) -0.0933(3) 0.2976(3) 0.079(3) Uani 1 1 d . . . H13D H 0.8720 -0.0787 0.3266 0.119 Uiso 1 1 calc R . . H13E H 0.8765 -0.1256 0.2912 0.119 Uiso 1 1 calc R . . H13F H 0.7938 -0.0988 0.3013 0.119 Uiso 1 1 calc R . . O103 O 0.7625(3) -0.09835(19) 0.21302(19) 0.0596(16) Uani 1 1 d . . . C134 C 0.7205(6) -0.1240(3) 0.1794(4) 0.099(4) Uani 1 1 d . . . H13G H 0.6749 -0.1403 0.1940 0.148 Uiso 1 1 calc R . . H13H H 0.7542 -0.1497 0.1649 0.148 Uiso 1 1 calc R . . H13I H 0.7025 -0.1003 0.1552 0.148 Uiso 1 1 calc R . . O104 O 0.9020(3) -0.10467(18) 0.1831(2) 0.0614(16) Uani 1 1 d . . . C135 C 0.9320(6) -0.1486(3) 0.2035(4) 0.108(4) Uani 1 1 d . . . H13J H 0.9692 -0.1646 0.1817 0.163 Uiso 1 1 calc R . . H13K H 0.8887 -0.1719 0.2102 0.163 Uiso 1 1 calc R . . H13L H 0.9592 -0.1401 0.2328 0.163 Uiso 1 1 calc R . . P102 P 1.00649(13) -0.23638(9) 0.30884(8) 0.0516(6) Uani 1 1 d D . . F101 F 0.9172(4) -0.2321(3) 0.3089(4) 0.242(6) Uani 1 1 d D . . F102 F 1.0006(5) -0.2283(3) 0.2564(2) 0.165(3) Uani 1 1 d D . . F103 F 1.0947(3) -0.2395(2) 0.3043(3) 0.178(4) Uani 1 1 d D . . F104 F 1.0014(3) -0.29522(18) 0.2991(2) 0.109(2) Uani 1 1 d D . . F105 F 1.0131(3) -0.17801(17) 0.31827(19) 0.0933(18) Uani 1 1 d D . . F106 F 1.0080(10) -0.2454(3) 0.3604(2) 0.290(8) Uani 1 1 d 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 0.0293(6) 0.0227(6) 0.0367(7) -0.0012(6) 0.0041(6) -0.0022(5) C1 0.113(8) 0.006(4) 0.049(6) 0.003(4) 0.036(6) 0.003(5) C2 0.082(7) 0.020(4) 0.044(6) 0.007(4) -0.019(5) -0.021(4) C3 0.042(5) 0.035(5) 0.043(6) 0.017(4) -0.005(4) -0.009(4) C4 0.056(6) 0.029(4) 0.038(5) 0.009(4) 0.014(4) 0.013(4) C5 0.047(5) 0.018(4) 0.060(6) 0.004(4) -0.011(5) 0.012(4) C6 0.044(6) 0.019(4) 0.081(7) 0.008(5) 0.017(5) 0.005(4) C7 0.189(11) 0.026(5) 0.061(7) -0.001(5) 0.056(7) 0.017(6) C8 0.182(11) 0.051(6) 0.088(8) 0.009(6) -0.060(8) -0.059(7) C9 0.037(5) 0.078(7) 0.139(9) 0.057(6) 0.004(6) -0.020(5) C10 0.109(8) 0.063(6) 0.044(6) 0.019(5) 0.013(5) 0.025(5) C11 0.074(7) 0.054(6) 0.109(8) -0.002(6) -0.049(6) 0.017(5) C12 0.053(6) 0.058(6) 0.166(11) 0.051(7) 0.057(6) 0.028(5) C13 0.027(4) 0.025(4) 0.029(5) 0.006(4) 0.000(4) 0.005(3) C14 0.022(4) 0.022(4) 0.043(5) -0.001(4) -0.002(3) -0.004(3) C15 0.030(4) 0.033(5) 0.039(5) 0.007(4) 0.006(4) -0.010(4) O1 0.043(3) 0.048(3) 0.055(4) -0.012(3) 0.015(3) -0.003(3) C21 0.028(4) 0.023(4) 0.037(5) 0.002(4) 0.011(4) -0.002(3) C22 0.034(5) 0.033(4) 0.046(5) -0.012(4) 0.001(4) -0.004(3) C23 0.032(5) 0.033(5) 0.060(6) 0.001(4) 0.005(5) -0.006(3) C24 0.036(5) 0.032(4) 0.050(6) 0.002(4) 0.014(4) 0.003(4) C25 0.047(5) 0.031(4) 0.038(5) 0.001(4) -0.001(4) 0.002(4) C26 0.029(4) 0.031(4) 0.042(5) 0.003(4) -0.007(4) 0.001(3) C27 0.025(4) 0.025(4) 0.031(5) -0.004(3) -0.004(3) 0.001(3) C28 0.034(4) 0.034(5) 0.031(5) -0.003(4) -0.004(3) -0.008(3) C29 0.038(5) 0.043(5) 0.026(4) -0.002(4) -0.001(4) 0.004(4) C30 0.033(5) 0.026(4) 0.042(5) -0.011(4) -0.011(4) 0.004(3) C31 0.036(5) 0.030(5) 0.045(6) 0.001(4) -0.001(4) -0.002(3) C32 0.037(5) 0.026(4) 0.036(5) -0.003(4) 0.004(4) 0.001(3) P1 0.0349(11) 0.0315(12) 0.0438(14) -0.0019(11) 0.0012(10) -0.0014(9) O2 0.063(3) 0.042(3) 0.027(3) -0.001(3) -0.004(3) -0.007(3) C33 0.116(8) 0.089(8) 0.043(6) -0.006(5) 0.012(6) -0.003(6) O3 0.069(4) 0.034(3) 0.064(4) 0.008(3) -0.014(3) 0.004(3) C34 0.104(8) 0.044(6) 0.098(8) -0.019(6) -0.017(6) 0.016(5) O4 0.027(3) 0.065(4) 0.068(4) 0.013(3) -0.003(3) -0.002(3) C35 0.039(6) 0.111(9) 0.121(9) 0.001(7) -0.009(6) 0.004(5) P2 0.0404(12) 0.0388(12) 0.0525(14) 0.0006(12) 0.0047(12) 0.0015(10) F1 0.130(5) 0.146(6) 0.104(5) 0.035(4) 0.073(4) 0.011(4) F2 0.080(3) 0.039(3) 0.155(5) 0.018(3) -0.034(3) 0.009(2) F3 0.070(3) 0.045(3) 0.096(4) 0.003(3) -0.006(3) 0.021(2) F4 0.059(3) 0.057(3) 0.144(5) 0.011(3) -0.036(3) -0.021(2) F5 0.103(4) 0.063(3) 0.067(3) 0.002(3) -0.036(3) -0.018(3) F6 0.054(3) 0.093(4) 0.069(4) -0.008(3) 0.014(3) 0.004(3) Cr2 0.0280(6) 0.0283(6) 0.0381(7) -0.0061(6) -0.0029(6) 0.0002(5) C101 0.036(5) 0.045(5) 0.060(6) -0.004(5) -0.001(4) -0.013(4) C102 0.031(4) 0.031(4) 0.052(6) 0.000(4) 0.001(4) 0.001(4) C103 0.025(4) 0.045(5) 0.048(6) -0.001(4) -0.009(4) -0.005(4) C104 0.038(5) 0.056(6) 0.037(5) -0.019(4) 0.000(4) -0.025(4) C105 0.037(5) 0.024(5) 0.087(8) -0.002(5) 0.009(5) -0.007(4) C106 0.025(4) 0.041(5) 0.073(7) 0.009(5) 0.005(5) -0.004(4) C107 0.065(6) 0.095(7) 0.049(6) 0.006(6) -0.009(5) -0.032(5) C108 0.036(5) 0.069(6) 0.081(7) -0.025(5) 0.009(5) 0.003(4) C109 0.041(5) 0.069(6) 0.071(6) 0.012(5) -0.019(4) -0.003(4) C110 0.061(6) 0.104(8) 0.074(7) -0.044(6) -0.008(5) -0.031(5) C111 0.071(6) 0.024(5) 0.176(11) -0.036(6) 0.038(7) -0.012(4) C112 0.055(6) 0.058(6) 0.157(10) 0.056(7) -0.025(6) 0.001(5) C113 0.029(4) 0.031(4) 0.023(4) 0.009(3) -0.003(3) 0.005(3) C114 0.028(4) 0.029(4) 0.031(5) 0.007(4) -0.002(3) 0.001(3) C115 0.022(4) 0.036(5) 0.045(5) 0.001(4) 0.006(4) 0.003(3) O101 0.047(3) 0.042(3) 0.050(4) -0.018(3) 0.000(3) -0.001(3) C121 0.025(4) 0.028(4) 0.040(5) -0.007(4) -0.001(4) -0.011(3) C122 0.042(5) 0.033(5) 0.040(5) -0.006(4) 0.000(4) 0.001(4) C123 0.052(5) 0.048(6) 0.042(5) -0.002(4) -0.006(4) -0.011(4) C124 0.053(6) 0.045(5) 0.049(6) -0.026(5) 0.012(5) -0.005(4) C125 0.049(5) 0.030(5) 0.048(6) -0.005(4) 0.012(4) 0.006(4) C126 0.031(4) 0.038(5) 0.047(5) 0.005(4) 0.005(4) 0.005(4) C127 0.021(4) 0.028(4) 0.032(5) -0.004(4) -0.001(3) 0.000(3) C128 0.041(5) 0.030(4) 0.043(5) -0.002(4) 0.003(4) -0.003(3) C129 0.033(5) 0.045(5) 0.067(7) 0.010(5) -0.005(5) -0.006(4) C130 0.033(5) 0.035(5) 0.078(7) 0.003(5) -0.023(5) -0.005(4) C131 0.050(5) 0.046(5) 0.048(6) 0.003(4) -0.021(5) -0.001(4) C132 0.029(4) 0.038(4) 0.034(5) 0.000(4) 0.001(4) -0.005(4) P101 0.0391(12) 0.0379(12) 0.0393(13) -0.0066(10) -0.0101(10) -0.0005(10) O102 0.073(4) 0.040(3) 0.044(4) 0.005(3) -0.015(3) 0.001(3) C133 0.115(8) 0.081(7) 0.043(6) 0.017(5) -0.014(6) -0.014(6) O103 0.067(4) 0.047(3) 0.064(4) 0.008(3) -0.023(3) -0.027(3) C134 0.101(8) 0.056(7) 0.139(10) 0.012(7) -0.054(8) -0.019(6) O104 0.060(4) 0.032(3) 0.092(5) 0.000(3) 0.001(3) 0.016(3) C135 0.108(9) 0.047(6) 0.171(12) 0.000(7) -0.005(8) 0.018(6) P102 0.0562(16) 0.0487(16) 0.0500(17) -0.0028(12) 0.0002(12) -0.0017(12) F101 0.098(5) 0.190(8) 0.436(17) -0.122(10) 0.144(8) -0.033(5) F102 0.264(9) 0.150(6) 0.079(5) 0.007(5) -0.060(5) 0.027(6) F103 0.057(4) 0.096(5) 0.380(13) -0.077(6) -0.091(5) 0.016(3) F104 0.131(5) 0.050(3) 0.147(6) -0.029(4) -0.023(4) -0.017(3) F105 0.125(4) 0.039(3) 0.116(5) -0.001(3) -0.010(4) 0.008(3) F106 0.73(3) 0.095(6) 0.043(4) 0.017(4) 0.015(9) -0.075(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 C15 1.832(8) . ? Cr1 C13 2.028(6) . ? Cr1 C14 2.067(6) . ? Cr1 C3 2.267(7) . ? Cr1 C4 2.276(7) . ? Cr1 C5 2.296(7) . ? Cr1 C6 2.298(7) . ? Cr1 P1 2.298(2) . ? Cr1 C2 2.311(7) . ? Cr1 C1 2.317(7) . ? C1 C2 1.412(11) . ? C1 C6 1.421(11) . ? C1 C7 1.496(10) . ? C2 C3 1.399(10) . ? C2 C8 1.526(10) . ? C3 C4 1.418(9) . ? C3 C9 1.503(9) . ? C4 C5 1.394(9) . ? C4 C10 1.513(9) . ? C5 C6 1.400(10) . ? C5 C11 1.521(10) . ? C6 C12 1.539(10) . ? C13 C14 1.269(8) . ? C13 C21 1.464(8) . ? C14 C27 1.456(8) . ? C15 O1 1.159(7) . ? C21 C26 1.396(9) . ? C21 C22 1.410(8) . ? C22 C23 1.390(9) . ? C23 C24 1.376(9) . ? C24 C25 1.372(9) . ? C25 C26 1.397(9) . ? C27 C28 1.391(9) . ? C27 C32 1.411(8) . ? C28 C29 1.392(8) . ? C29 C30 1.370(9) . ? C30 C31 1.377(9) . ? C31 C32 1.380(9) . ? P1 O2 1.580(5) . ? P1 O4 1.582(5) . ? P1 O3 1.605(5) . ? O2 C33 1.427(9) . ? O3 C34 1.425(8) . ? O4 C35 1.425(9) . ? P2 F1 1.549(5) . ? P2 F5 1.571(5) . ? P2 F2 1.577(4) . ? P2 F6 1.594(5) . ? P2 F4 1.596(5) . ? P2 F3 1.601(4) . ? Cr2 C115 1.822(8) . ? Cr2 C113 2.023(6) . ? Cr2 C114 2.056(6) . ? Cr2 C102 2.264(7) . ? Cr2 C101 2.275(8) . ? Cr2 P101 2.289(2) . ? Cr2 C104 2.294(7) . ? Cr2 C105 2.296(7) . ? Cr2 C106 2.309(7) . ? Cr2 C103 2.328(6) . ? C101 C106 1.391(10) . ? C101 C102 1.441(10) . ? C101 C107 1.508(10) . ? C102 C103 1.375(9) . ? C102 C108 1.534(9) . ? C103 C104 1.441(10) . ? C103 C109 1.517(9) . ? C104 C105 1.437(10) . ? C104 C110 1.513(10) . ? C105 C106 1.382(11) . ? C105 C111 1.521(10) . ? C106 C112 1.533(10) . ? C113 C114 1.267(8) . ? C113 C121 1.481(9) . ? C114 C127 1.465(8) . ? C115 O101 1.167(7) . ? C121 C122 1.382(9) . ? C121 C126 1.403(9) . ? C122 C123 1.391(9) . ? C123 C124 1.394(10) . ? C124 C125 1.377(10) . ? C125 C126 1.373(9) . ? C127 C132 1.391(8) . ? C127 C128 1.399(8) . ? C128 C129 1.380(9) . ? C129 C130 1.387(10) . ? C130 C131 1.385(9) . ? C131 C132 1.383(8) . ? P101 O102 1.570(5) . ? P101 O103 1.574(5) . ? P101 O104 1.595(5) . ? O102 C133 1.455(8) . ? O103 C134 1.373(9) . ? O104 C135 1.397(9) . ? P102 F106 1.485(6) . ? P102 F103 1.508(5) . ? P102 F102 1.510(6) . ? P102 F101 1.521(7) . ? P102 F105 1.574(5) . ? P102 F104 1.587(5) . ? 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 C15 Cr1 C13 110.0(3) . . ? C15 Cr1 C14 77.0(3) . . ? C13 Cr1 C14 36.1(2) . . ? C15 Cr1 C3 90.0(3) . . ? C13 Cr1 C3 159.0(3) . . ? C14 Cr1 C3 154.9(3) . . ? C15 Cr1 C4 82.4(3) . . ? C13 Cr1 C4 137.1(3) . . ? C14 Cr1 C4 119.4(3) . . ? C3 Cr1 C4 36.4(2) . . ? C15 Cr1 C5 104.3(3) . . ? C13 Cr1 C5 102.6(3) . . ? C14 Cr1 C5 97.4(3) . . ? C3 Cr1 C5 64.7(3) . . ? C4 Cr1 C5 35.5(2) . . ? C15 Cr1 C6 139.6(3) . . ? C13 Cr1 C6 84.3(2) . . ? C14 Cr1 C6 100.2(3) . . ? C3 Cr1 C6 75.9(3) . . ? C4 Cr1 C6 63.7(3) . . ? C5 Cr1 C6 35.5(3) . . ? C15 Cr1 P1 86.1(2) . . ? C13 Cr1 P1 87.53(19) . . ? C14 Cr1 P1 99.64(19) . . ? C3 Cr1 P1 100.8(2) . . ? C4 Cr1 P1 135.1(2) . . ? C5 Cr1 P1 161.68(19) . . ? C6 Cr1 P1 133.3(3) . . ? C15 Cr1 C2 121.4(3) . . ? C13 Cr1 C2 127.6(3) . . ? C14 Cr1 C2 161.2(3) . . ? C3 Cr1 C2 35.6(3) . . ? C4 Cr1 C2 64.0(3) . . ? C5 Cr1 C2 75.3(3) . . ? C6 Cr1 C2 63.8(3) . . ? P1 Cr1 C2 86.4(2) . . ? C15 Cr1 C1 154.3(3) . . ? C13 Cr1 C1 95.3(3) . . ? C14 Cr1 C1 125.7(3) . . ? C3 Cr1 C1 64.5(3) . . ? C4 Cr1 C1 75.8(3) . . ? C5 Cr1 C1 64.3(3) . . ? C6 Cr1 C1 35.9(3) . . ? P1 Cr1 C1 99.9(3) . . ? C2 Cr1 C1 35.5(3) . . ? C2 C1 C6 118.4(7) . . ? C2 C1 C7 119.7(10) . . ? C6 C1 C7 121.8(9) . . ? C2 C1 Cr1 72.0(4) . . ? C6 C1 Cr1 71.3(4) . . ? C7 C1 Cr1 131.1(5) . . ? C3 C2 C1 120.9(7) . . ? C3 C2 C8 117.9(8) . . ? C1 C2 C8 121.0(9) . . ? C3 C2 Cr1 70.5(4) . . ? C1 C2 Cr1 72.5(4) . . ? C8 C2 Cr1 135.0(5) . . ? C2 C3 C4 119.4(7) . . ? C2 C3 C9 120.8(8) . . ? C4 C3 C9 119.7(8) . . ? C2 C3 Cr1 73.9(4) . . ? C4 C3 Cr1 72.1(4) . . ? C9 C3 Cr1 128.8(5) . . ? C5 C4 C3 120.6(7) . . ? C5 C4 C10 119.2(8) . . ? C3 C4 C10 120.1(7) . . ? C5 C4 Cr1 73.0(4) . . ? C3 C4 Cr1 71.5(4) . . ? C10 C4 Cr1 132.0(5) . . ? C4 C5 C6 119.6(7) . . ? C4 C5 C11 120.7(8) . . ? C6 C5 C11 119.7(8) . . ? C4 C5 Cr1 71.5(4) . . ? C6 C5 Cr1 72.3(4) . . ? C11 C5 Cr1 129.4(5) . . ? C5 C6 C1 121.0(7) . . ? C5 C6 C12 119.1(8) . . ? C1 C6 C12 119.7(9) . . ? C5 C6 Cr1 72.2(4) . . ? C1 C6 Cr1 72.8(4) . . ? C12 C6 Cr1 132.1(5) . . ? C14 C13 C21 142.2(6) . . ? C14 C13 Cr1 73.6(4) . . ? C21 C13 Cr1 143.5(5) . . ? C13 C14 C27 145.7(6) . . ? C13 C14 Cr1 70.3(4) . . ? C27 C14 Cr1 144.0(5) . . ? O1 C15 Cr1 177.5(6) . . ? C26 C21 C22 118.5(6) . . ? C26 C21 C13 122.1(6) . . ? C22 C21 C13 119.4(6) . . ? C23 C22 C21 120.5(7) . . ? C24 C23 C22 119.8(7) . . ? C25 C24 C23 120.8(7) . . ? C24 C25 C26 120.3(7) . . ? C21 C26 C25 120.1(6) . . ? C28 C27 C32 117.6(6) . . ? C28 C27 C14 123.4(6) . . ? C32 C27 C14 118.9(6) . . ? C27 C28 C29 120.9(6) . . ? C30 C29 C28 120.5(7) . . ? C29 C30 C31 119.8(7) . . ? C30 C31 C32 120.6(7) . . ? C31 C32 C27 120.7(7) . . ? O2 P1 O4 106.7(3) . . ? O2 P1 O3 98.6(3) . . ? O4 P1 O3 106.4(3) . . ? O2 P1 Cr1 115.4(2) . . ? O4 P1 Cr1 109.1(2) . . ? O3 P1 Cr1 119.5(2) . . ? C33 O2 P1 127.0(5) . . ? C34 O3 P1 122.1(5) . . ? C35 O4 P1 128.2(5) . . ? F1 P2 F5 91.9(3) . . ? F1 P2 F2 91.0(3) . . ? F5 P2 F2 90.0(3) . . ? F1 P2 F6 178.1(3) . . ? F5 P2 F6 88.8(3) . . ? F2 P2 F6 90.8(3) . . ? F1 P2 F4 90.3(3) . . ? F5 P2 F4 177.8(3) . . ? F2 P2 F4 90.2(3) . . ? F6 P2 F4 89.1(3) . . ? F1 P2 F3 91.0(3) . . ? F5 P2 F3 90.5(3) . . ? F2 P2 F3 177.9(3) . . ? F6 P2 F3 87.2(3) . . ? F4 P2 F3 89.2(3) . . ? C115 Cr2 C113 109.4(3) . . ? C115 Cr2 C114 75.3(3) . . ? C113 Cr2 C114 36.2(2) . . ? C115 Cr2 C102 86.8(3) . . ? C113 Cr2 C102 160.9(3) . . ? C114 Cr2 C102 151.5(3) . . ? C115 Cr2 C101 82.3(3) . . ? C113 Cr2 C101 132.8(3) . . ? C114 Cr2 C101 117.1(3) . . ? C102 Cr2 C101 37.0(2) . . ? C115 Cr2 P101 85.1(2) . . ? C113 Cr2 P101 87.60(18) . . ? C114 Cr2 P101 96.30(18) . . ? C102 Cr2 P101 104.21(19) . . ? C101 Cr2 P101 139.6(2) . . ? C115 Cr2 C104 151.3(3) . . ? C113 Cr2 C104 99.2(3) . . ? C114 Cr2 C104 132.1(3) . . ? C102 Cr2 C104 64.6(3) . . ? C101 Cr2 C104 76.8(3) . . ? P101 Cr2 C104 98.1(2) . . ? C115 Cr2 C105 142.5(3) . . ? C113 Cr2 C105 85.1(3) . . ? C114 Cr2 C105 105.3(3) . . ? C102 Cr2 C105 75.8(3) . . ? C101 Cr2 C105 63.7(3) . . ? P101 Cr2 C105 131.0(3) . . ? C104 Cr2 C105 36.5(3) . . ? C115 Cr2 C106 107.6(3) . . ? C113 Cr2 C106 100.0(3) . . ? C114 Cr2 C106 99.7(3) . . ? C102 Cr2 C106 64.5(3) . . ? C101 Cr2 C106 35.3(3) . . ? P101 Cr2 C106 161.7(2) . . ? C104 Cr2 C106 64.4(3) . . ? C105 Cr2 C106 34.9(3) . . ? C115 Cr2 C103 116.0(3) . . ? C113 Cr2 C103 133.6(3) . . ? C114 Cr2 C103 168.4(3) . . ? C102 Cr2 C103 34.8(2) . . ? C101 Cr2 C103 64.4(3) . . ? P101 Cr2 C103 87.60(19) . . ? C104 Cr2 C103 36.3(2) . . ? C105 Cr2 C103 64.4(3) . . ? C106 Cr2 C103 75.1(3) . . ? C106 C101 C102 118.9(7) . . ? C106 C101 C107 120.5(8) . . ? C102 C101 C107 120.5(7) . . ? C106 C101 Cr2 73.7(4) . . ? C102 C101 Cr2 71.1(4) . . ? C107 C101 Cr2 129.9(5) . . ? C103 C102 C101 121.1(7) . . ? C103 C102 C108 120.9(7) . . ? C101 C102 C108 117.9(7) . . ? C103 C102 Cr2 75.1(4) . . ? C101 C102 Cr2 71.9(4) . . ? C108 C102 Cr2 128.4(5) . . ? C102 C103 C104 119.8(7) . . ? C102 C103 C109 120.9(7) . . ? C104 C103 C109 119.2(7) . . ? C102 C103 Cr2 70.1(4) . . ? C104 C103 Cr2 70.6(4) . . ? C109 C103 Cr2 134.5(5) . . ? C105 C104 C103 117.9(7) . . ? C105 C104 C110 122.2(8) . . ? C103 C104 C110 119.7(8) . . ? C105 C104 Cr2 71.8(4) . . ? C103 C104 Cr2 73.1(4) . . ? C110 C104 Cr2 130.2(5) . . ? C106 C105 C104 121.0(7) . . ? C106 C105 C111 120.8(8) . . ? C104 C105 C111 117.9(9) . . ? C106 C105 Cr2 73.0(4) . . ? C104 C105 Cr2 71.7(4) . . ? C111 C105 Cr2 133.5(5) . . ? C105 C106 C101 121.0(8) . . ? C105 C106 C112 118.8(8) . . ? C101 C106 C112 120.3(8) . . ? C105 C106 Cr2 72.0(4) . . ? C101 C106 Cr2 71.0(4) . . ? C112 C106 Cr2 129.4(5) . . ? C114 C113 C121 143.6(6) . . ? C114 C113 Cr2 73.4(4) . . ? C121 C113 Cr2 142.2(5) . . ? C113 C114 C127 142.4(6) . . ? C113 C114 Cr2 70.5(4) . . ? C127 C114 Cr2 147.0(5) . . ? O101 C115 Cr2 178.5(6) . . ? C122 C121 C126 118.8(7) . . ? C122 C121 C113 122.1(6) . . ? C126 C121 C113 119.2(7) . . ? C121 C122 C123 120.4(7) . . ? C122 C123 C124 120.4(7) . . ? C125 C124 C123 118.7(7) . . ? C126 C125 C124 121.3(7) . . ? C125 C126 C121 120.3(7) . . ? C132 C127 C128 120.0(6) . . ? C132 C127 C114 122.2(6) . . ? C128 C127 C114 117.8(6) . . ? C129 C128 C127 119.6(7) . . ? C128 C129 C130 121.1(7) . . ? C129 C130 C131 118.6(7) . . ? C132 C131 C130 121.7(7) . . ? C131 C132 C127 119.0(6) . . ? O102 P101 O103 99.6(3) . . ? O102 P101 O104 107.2(3) . . ? O103 P101 O104 105.6(3) . . ? O102 P101 Cr2 117.7(2) . . ? O103 P101 Cr2 119.5(2) . . ? O104 P101 Cr2 106.2(2) . . ? C133 O102 P101 127.2(5) . . ? C134 O103 P101 127.4(6) . . ? C135 O104 P101 126.8(6) . . ? F106 P102 F103 93.4(7) . . ? F106 P102 F102 176.9(7) . . ? F103 P102 F102 89.3(5) . . ? F106 P102 F101 91.6(7) . . ? F103 P102 F101 175.0(6) . . ? F102 P102 F101 85.7(6) . . ? F106 P102 F105 89.4(4) . . ? F103 P102 F105 89.9(3) . . ? F102 P102 F105 92.0(4) . . ? F101 P102 F105 89.9(4) . . ? F106 P102 F104 90.8(4) . . ? F103 P102 F104 89.2(3) . . ? F102 P102 F104 87.9(4) . . ? F101 P102 F104 91.1(4) . . ? F105 P102 F104 179.0(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.722 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.077 #===END data_7plus _database_code_CSD 189056 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H41 Cr F6 N O3 P' _chemical_formula_weight 756.69 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' 'F' 'F' 0.0171 0.0103 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1760(17) _cell_length_b 22.284(5) _cell_length_c 14.739(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.917(12) _cell_angle_gamma 90.00 _cell_volume 3547.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 254 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red-black _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1572 _exptl_absorpt_coefficient_mu 0.437 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9785 _exptl_absorpt_correction_T_max 0.9785 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _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 with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 18328 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6232 _reflns_number_gt 4786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+8.3537P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6232 _refine_ls_number_parameters 506 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.157 _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 0.43322(5) 0.11446(3) 0.60917(4) 0.02255(16) Uani 1 1 d . . . C1 C 0.6015(4) 0.10088(19) 0.7336(3) 0.0347(10) Uani 1 1 d . . . C2 C 0.5623(4) 0.1616(2) 0.7335(3) 0.0391(10) Uani 1 1 d . . . C3 C 0.4393(5) 0.17348(19) 0.7387(3) 0.0424(12) Uani 1 1 d . . . C4 C 0.3550(4) 0.1252(2) 0.7353(3) 0.0412(11) Uani 1 1 d . . . C5 C 0.3952(4) 0.0665(2) 0.7335(3) 0.0386(10) Uani 1 1 d . . . C6 C 0.5208(4) 0.05486(19) 0.7358(3) 0.0401(10) Uani 1 1 d . . . C7 C 0.7353(4) 0.0879(3) 0.7347(4) 0.0672(17) Uani 1 1 d . . . H7A H 0.7850 0.0846 0.7998 0.101 Uiso 1 1 calc R . . H7B H 0.7675 0.1207 0.7034 0.101 Uiso 1 1 calc R . . H7C H 0.7398 0.0502 0.7017 0.101 Uiso 1 1 calc R . . C8 C 0.6510(6) 0.2129(3) 0.7349(4) 0.0682(17) Uani 1 1 d . . . H8A H 0.6931 0.2228 0.8001 0.102 Uiso 1 1 calc R . . H8B H 0.6050 0.2480 0.7043 0.102 Uiso 1 1 calc R . . H8C H 0.7124 0.2011 0.7013 0.102 Uiso 1 1 calc R . . C9 C 0.3996(6) 0.2361(2) 0.7541(4) 0.0715(18) Uani 1 1 d . . . H9A H 0.4191 0.2444 0.8216 0.107 Uiso 1 1 calc R . . H9B H 0.3102 0.2400 0.7270 0.107 Uiso 1 1 calc R . . H9C H 0.4435 0.2647 0.7237 0.107 Uiso 1 1 calc R . . C10 C 0.2203(5) 0.1382(3) 0.7310(4) 0.0704(18) Uani 1 1 d . . . H10A H 0.2098 0.1407 0.7948 0.106 Uiso 1 1 calc R . . H10B H 0.1682 0.1058 0.6969 0.106 Uiso 1 1 calc R . . H10C H 0.1960 0.1763 0.6984 0.106 Uiso 1 1 calc R . . C11 C 0.3103(5) 0.0135(3) 0.7373(4) 0.0664(16) Uani 1 1 d . . . H11A H 0.3150 0.0036 0.8029 0.100 Uiso 1 1 calc R . . H11B H 0.3363 -0.0213 0.7064 0.100 Uiso 1 1 calc R . . H11C H 0.2248 0.0241 0.7049 0.100 Uiso 1 1 calc R . . C12 C 0.5680(6) -0.0098(2) 0.7402(4) 0.0739(18) Uani 1 1 d . . . H12A H 0.6000 -0.0219 0.8060 0.111 Uiso 1 1 calc R . . H12B H 0.6343 -0.0126 0.7080 0.111 Uiso 1 1 calc R . . H12C H 0.4998 -0.0365 0.7095 0.111 Uiso 1 1 calc R . . C13 C 0.3138(3) 0.17545(16) 0.5316(2) 0.0250(8) Uani 1 1 d . . . C14 C 0.2695(3) 0.12406(16) 0.5032(2) 0.0250(8) Uani 1 1 d . . . C15 C 0.4029(3) 0.04112(18) 0.5503(3) 0.0290(9) Uani 1 1 d . . . O1 O 0.3782(3) -0.00588(12) 0.5186(2) 0.0397(7) Uani 1 1 d . . . C16 C 0.5447(3) 0.13712(16) 0.5316(3) 0.0259(8) Uani 1 1 d . . . N1 N 0.6051(3) 0.14989(14) 0.4816(2) 0.0309(7) Uani 1 1 d . . . C21 C 0.2907(3) 0.23939(17) 0.5177(2) 0.0254(8) Uani 1 1 d . . . C22 C 0.1703(3) 0.26146(17) 0.5052(2) 0.0276(8) Uani 1 1 d . . . H22A H 0.1052 0.2346 0.5076 0.033 Uiso 1 1 calc R . . C23 C 0.1449(4) 0.32215(17) 0.4894(3) 0.0292(9) Uani 1 1 d . . . H23A H 0.0631 0.3367 0.4822 0.035 Uiso 1 1 calc R . . C24 C 0.2388(4) 0.36119(17) 0.4841(3) 0.0288(8) Uani 1 1 d . . . C25 C 0.3588(4) 0.33959(17) 0.4945(3) 0.0304(9) Uani 1 1 d . . . H25A H 0.4230 0.3663 0.4892 0.037 Uiso 1 1 calc R . . C26 C 0.3844(3) 0.27957(17) 0.5124(3) 0.0285(8) Uani 1 1 d . . . H26A H 0.4667 0.2654 0.5212 0.034 Uiso 1 1 calc R . . O2 O 0.2233(3) 0.42159(12) 0.4690(2) 0.0399(7) Uani 1 1 d . . . C33 C 0.1131(4) 0.4481(2) 0.4827(3) 0.0438(11) Uani 1 1 d . . . H33A H 0.1133 0.4912 0.4697 0.066 Uiso 1 1 calc R . . H33B H 0.1096 0.4418 0.5478 0.066 Uiso 1 1 calc R . . H33C H 0.0408 0.4294 0.4400 0.066 Uiso 1 1 calc R . . C27 C 0.1838(3) 0.09198(16) 0.4276(3) 0.0252(8) Uani 1 1 d . . . C28 C 0.1655(3) 0.11178(17) 0.3355(3) 0.0266(8) Uani 1 1 d . . . H28A H 0.2027 0.1484 0.3243 0.032 Uiso 1 1 calc R . . C29 C 0.0951(3) 0.08011(18) 0.2597(3) 0.0293(9) Uani 1 1 d . . . H29A H 0.0852 0.0944 0.1974 0.035 Uiso 1 1 calc R . . C30 C 0.0388(3) 0.02690(18) 0.2762(3) 0.0298(9) Uani 1 1 d . . . C31 C 0.0504(4) 0.00787(17) 0.3676(3) 0.0311(9) Uani 1 1 d . . . H31A H 0.0078 -0.0271 0.3789 0.037 Uiso 1 1 calc R . . C32 C 0.1229(3) 0.03915(17) 0.4420(3) 0.0297(9) Uani 1 1 d . . . H32A H 0.1320 0.0248 0.5041 0.036 Uiso 1 1 calc R . . O3 O -0.0280(3) -0.00983(13) 0.20821(19) 0.0400(7) Uani 1 1 d . . . C34 C -0.0350(5) 0.0050(2) 0.1131(3) 0.0603(15) Uani 1 1 d . . . H34A H -0.0857 -0.0249 0.0716 0.091 Uiso 1 1 calc R . . H34B H 0.0485 0.0053 0.1033 0.091 Uiso 1 1 calc R . . H34C H -0.0726 0.0447 0.0988 0.091 Uiso 1 1 calc R . . C35 C 0.6608(4) 0.15161(17) 0.4060(3) 0.0291(9) Uani 1 1 d . . . C36 C 0.7864(4) 0.14043(17) 0.4234(3) 0.0345(9) Uani 1 1 d . . . C37 C 0.8340(4) 0.13467(18) 0.3453(3) 0.0388(10) Uani 1 1 d . . . H37A H 0.9194 0.1259 0.3538 0.047 Uiso 1 1 calc R . . C38 C 0.7586(4) 0.14153(19) 0.2556(3) 0.0384(10) Uani 1 1 d . . . H38A H 0.7917 0.1356 0.2030 0.046 Uiso 1 1 calc R . . C39 C 0.6361(4) 0.1569(2) 0.2418(3) 0.0404(10) Uani 1 1 d . . . H39A H 0.5864 0.1636 0.1798 0.049 Uiso 1 1 calc R . . C40 C 0.5845(4) 0.1628(2) 0.3173(3) 0.0380(10) Uani 1 1 d . . . C41 C 0.8663(4) 0.1359(2) 0.5215(3) 0.0543(13) Uani 1 1 d . . . H41A H 0.8153 0.1413 0.5660 0.082 Uiso 1 1 calc R . . H41B H 0.9301 0.1671 0.5319 0.082 Uiso 1 1 calc R . . H41C H 0.9058 0.0963 0.5309 0.082 Uiso 1 1 calc R . . C42 C 0.4503(4) 0.1797(3) 0.3040(3) 0.0625(16) Uani 1 1 d . . . H42A H 0.4115 0.1859 0.2371 0.094 Uiso 1 1 calc R . . H42B H 0.4450 0.2169 0.3384 0.094 Uiso 1 1 calc R . . H42C H 0.4072 0.1475 0.3279 0.094 Uiso 1 1 calc R . . P1 P 0.26176(11) 0.15311(6) 0.01780(8) 0.0463(3) Uani 1 1 d D . . F1 F 0.1385(6) 0.1667(5) -0.0601(5) 0.086(4) Uani 0.548(11) 1 d PD A 1 F2 F 0.2336(14) 0.2005(5) 0.0819(8) 0.111(5) Uani 0.548(11) 1 d PD A 1 F3 F 0.2833(9) 0.1013(3) -0.0544(6) 0.069(3) Uani 0.548(11) 1 d PD A 1 F4 F 0.3845(9) 0.1300(6) 0.0864(8) 0.077(3) Uani 0.548(11) 1 d PD A 1 F5 F 0.3342(7) 0.1953(3) -0.0322(8) 0.086(3) Uani 0.548(11) 1 d PD A 1 F6 F 0.1878(9) 0.1034(5) 0.0586(5) 0.118(4) Uani 0.548(11) 1 d PD A 1 F1' F 0.1836(12) 0.2019(6) -0.0465(8) 0.124(5) Uani 0.452(11) 1 d PD A 2 F2' F 0.2071(13) 0.1762(7) 0.1024(9) 0.086(4) Uani 0.452(11) 1 d PD A 2 F3' F 0.3301(10) 0.1316(10) -0.0530(8) 0.163(11) Uani 0.452(11) 1 d PD A 2 F4' F 0.3444(14) 0.1124(6) 0.0957(12) 0.095(5) Uani 0.452(11) 1 d PD A 2 F5' F 0.3681(8) 0.2034(4) 0.0556(10) 0.100(4) Uani 0.452(11) 1 d PD A 2 F6' F 0.1607(10) 0.1084(5) -0.0074(13) 0.174(9) Uani 0.452(11) 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 0.0246(3) 0.0221(3) 0.0216(3) -0.0008(2) 0.0073(2) 0.0023(2) C1 0.030(2) 0.048(3) 0.024(2) 0.0031(18) 0.0044(16) 0.0075(19) C2 0.050(3) 0.040(2) 0.024(2) 0.0003(18) 0.0031(19) -0.016(2) C3 0.074(3) 0.032(2) 0.0172(19) 0.0000(16) 0.006(2) 0.022(2) C4 0.032(2) 0.072(3) 0.021(2) 0.001(2) 0.0093(17) 0.009(2) C5 0.043(3) 0.050(3) 0.021(2) 0.0064(18) 0.0056(18) -0.011(2) C6 0.056(3) 0.032(2) 0.029(2) 0.0037(18) 0.0043(19) 0.009(2) C7 0.039(3) 0.116(5) 0.047(3) 0.011(3) 0.011(2) 0.022(3) C8 0.085(4) 0.068(4) 0.044(3) -0.002(3) 0.004(3) -0.044(3) C9 0.122(5) 0.047(3) 0.041(3) -0.004(2) 0.014(3) 0.034(3) C10 0.041(3) 0.130(6) 0.043(3) -0.001(3) 0.014(2) 0.024(3) C11 0.070(4) 0.074(4) 0.055(3) 0.012(3) 0.016(3) -0.034(3) C12 0.110(5) 0.040(3) 0.061(3) 0.005(3) 0.003(3) 0.026(3) C13 0.0253(19) 0.029(2) 0.0215(18) 0.0017(15) 0.0074(15) 0.0038(16) C14 0.0245(19) 0.029(2) 0.0234(18) 0.0006(15) 0.0090(15) 0.0014(16) C15 0.027(2) 0.032(2) 0.030(2) 0.0040(17) 0.0103(16) 0.0069(17) O1 0.0401(18) 0.0259(16) 0.0536(19) -0.0123(14) 0.0132(14) -0.0003(13) C16 0.0235(19) 0.0248(19) 0.0273(19) -0.0030(15) 0.0025(16) 0.0036(16) N1 0.0300(18) 0.0306(18) 0.0351(18) -0.0013(14) 0.0140(15) 0.0002(14) C21 0.027(2) 0.030(2) 0.0194(17) -0.0035(15) 0.0058(15) 0.0035(16) C22 0.025(2) 0.033(2) 0.0243(19) -0.0007(16) 0.0043(15) -0.0021(16) C23 0.029(2) 0.033(2) 0.025(2) -0.0013(16) 0.0046(16) 0.0061(17) C24 0.034(2) 0.026(2) 0.0263(19) -0.0024(16) 0.0063(16) 0.0042(17) C25 0.030(2) 0.027(2) 0.035(2) -0.0008(17) 0.0084(17) -0.0024(17) C26 0.025(2) 0.031(2) 0.030(2) -0.0035(16) 0.0078(16) 0.0022(16) O2 0.0409(17) 0.0261(15) 0.0523(18) 0.0012(13) 0.0114(14) 0.0074(13) C33 0.050(3) 0.036(2) 0.045(3) -0.002(2) 0.010(2) 0.017(2) C27 0.0228(19) 0.0247(19) 0.0282(19) -0.0012(15) 0.0068(15) 0.0030(15) C28 0.0220(18) 0.0255(19) 0.033(2) 0.0047(16) 0.0090(15) 0.0016(16) C29 0.025(2) 0.037(2) 0.0257(19) 0.0066(16) 0.0060(16) -0.0005(17) C30 0.0236(19) 0.034(2) 0.030(2) -0.0030(17) 0.0029(16) -0.0006(17) C31 0.029(2) 0.028(2) 0.037(2) 0.0030(17) 0.0087(17) -0.0042(17) C32 0.031(2) 0.033(2) 0.027(2) 0.0039(16) 0.0099(16) -0.0009(17) O3 0.0421(17) 0.0424(17) 0.0309(15) -0.0054(13) 0.0009(13) -0.0133(14) C34 0.073(4) 0.066(3) 0.031(3) -0.007(2) -0.006(2) -0.021(3) C35 0.032(2) 0.025(2) 0.036(2) -0.0020(16) 0.0199(18) -0.0037(16) C36 0.039(2) 0.024(2) 0.045(2) 0.0098(18) 0.021(2) 0.0033(18) C37 0.039(2) 0.028(2) 0.059(3) 0.0069(19) 0.030(2) 0.0020(18) C38 0.044(3) 0.036(2) 0.044(2) -0.0056(19) 0.028(2) -0.010(2) C39 0.040(2) 0.050(3) 0.034(2) -0.010(2) 0.0142(19) -0.014(2) C40 0.035(2) 0.047(3) 0.036(2) -0.0101(19) 0.0145(19) -0.0057(19) C41 0.041(3) 0.070(3) 0.056(3) 0.025(3) 0.019(2) 0.016(2) C42 0.031(3) 0.119(5) 0.038(3) -0.009(3) 0.009(2) 0.003(3) P1 0.0343(6) 0.0643(8) 0.0405(7) -0.0015(6) 0.0100(5) -0.0003(6) F1 0.033(3) 0.175(11) 0.049(4) -0.020(5) 0.007(3) 0.027(5) F2 0.153(12) 0.103(8) 0.075(7) -0.051(7) 0.023(6) 0.038(7) F3 0.090(8) 0.069(5) 0.049(4) -0.001(3) 0.020(5) 0.023(4) F4 0.050(4) 0.111(10) 0.057(5) -0.012(5) -0.009(4) 0.011(5) F5 0.080(6) 0.062(4) 0.126(9) 0.015(5) 0.047(5) -0.017(4) F6 0.120(8) 0.177(10) 0.069(5) 0.010(6) 0.048(5) -0.070(7) F1' 0.126(12) 0.130(11) 0.089(8) 0.044(7) -0.022(7) 0.046(9) F2' 0.071(6) 0.130(12) 0.059(6) -0.005(7) 0.023(5) 0.026(7) F3' 0.051(8) 0.40(3) 0.042(5) -0.030(13) 0.014(5) 0.072(13) F4' 0.125(14) 0.052(7) 0.093(7) 0.015(5) 0.004(9) 0.028(8) F5' 0.076(6) 0.085(6) 0.133(11) 0.009(6) 0.019(6) -0.033(5) F6' 0.089(8) 0.115(12) 0.30(2) -0.122(15) 0.014(13) -0.050(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C15 1.840(4) . ? Cr1 C16 1.962(4) . ? Cr1 C13 2.037(4) . ? Cr1 C14 2.088(4) . ? Cr1 C5 2.255(4) . ? Cr1 C4 2.262(4) . ? Cr1 C2 2.276(4) . ? Cr1 C1 2.284(4) . ? Cr1 C6 2.295(4) . ? Cr1 C3 2.305(4) . ? C1 C6 1.371(6) . ? C1 C2 1.423(6) . ? C1 C7 1.520(6) . ? C2 C3 1.420(7) . ? C2 C8 1.509(6) . ? C3 C4 1.423(7) . ? C3 C9 1.499(6) . ? C4 C5 1.386(6) . ? C4 C10 1.517(6) . ? C5 C6 1.419(6) . ? C5 C11 1.525(6) . ? C6 C12 1.531(6) . ? C13 C14 1.275(5) . ? C13 C21 1.453(5) . ? C14 C27 1.457(5) . ? C15 O1 1.151(5) . ? C16 N1 1.156(5) . ? N1 C35 1.410(5) . ? C21 C26 1.395(5) . ? C21 C22 1.399(5) . ? C22 C23 1.389(5) . ? C23 C24 1.381(5) . ? C24 O2 1.368(5) . ? C24 C25 1.396(5) . ? C25 C26 1.379(5) . ? O2 C33 1.426(5) . ? C27 C28 1.392(5) . ? C27 C32 1.403(5) . ? C28 C29 1.383(5) . ? C29 C30 1.393(5) . ? C30 O3 1.359(4) . ? C30 C31 1.386(5) . ? C31 C32 1.374(5) . ? O3 C34 1.423(5) . ? C35 C36 1.383(6) . ? C35 C40 1.387(6) . ? C36 C37 1.393(6) . ? C36 C41 1.494(6) . ? C37 C38 1.381(6) . ? C38 C39 1.375(6) . ? C39 C40 1.386(6) . ? C40 C42 1.510(6) . ? P1 F6' 1.479(9) . ? P1 F2 1.503(8) . ? P1 F3' 1.521(9) . ? P1 F5 1.546(6) . ? P1 F1' 1.554(9) . ? P1 F4' 1.565(11) . ? P1 F4 1.567(9) . ? P1 F1 1.579(6) . ? P1 F6 1.589(7) . ? P1 F2' 1.608(10) . ? P1 F5' 1.624(8) . ? P1 F3 1.631(8) . ? 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 C15 Cr1 C16 91.24(16) . . ? C15 Cr1 C13 108.26(16) . . ? C16 Cr1 C13 85.61(15) . . ? C15 Cr1 C14 73.68(15) . . ? C16 Cr1 C14 95.94(14) . . ? C13 Cr1 C14 35.96(14) . . ? C15 Cr1 C5 84.93(16) . . ? C16 Cr1 C5 151.26(16) . . ? C13 Cr1 C5 122.64(16) . . ? C14 Cr1 C5 110.13(15) . . ? C15 Cr1 C4 114.70(18) . . ? C16 Cr1 C4 152.86(17) . . ? C13 Cr1 C4 93.15(15) . . ? C14 Cr1 C4 98.86(14) . . ? C5 Cr1 C4 35.73(17) . . ? C15 Cr1 C2 142.30(17) . . ? C16 Cr1 C2 89.11(15) . . ? C13 Cr1 C2 109.36(16) . . ? C14 Cr1 C2 143.71(16) . . ? C5 Cr1 C2 77.15(15) . . ? C4 Cr1 C2 65.70(16) . . ? C15 Cr1 C1 105.93(16) . . ? C16 Cr1 C1 89.26(15) . . ? C13 Cr1 C1 145.51(15) . . ? C14 Cr1 C1 174.79(15) . . ? C5 Cr1 C1 64.72(15) . . ? C4 Cr1 C1 76.51(15) . . ? C2 Cr1 C1 36.37(16) . . ? C15 Cr1 C6 81.81(16) . . ? C16 Cr1 C6 114.92(16) . . ? C13 Cr1 C6 157.43(15) . . ? C14 Cr1 C6 140.87(16) . . ? C5 Cr1 C6 36.34(16) . . ? C4 Cr1 C6 64.33(16) . . ? C2 Cr1 C6 64.12(15) . . ? C1 Cr1 C6 34.86(15) . . ? C15 Cr1 C3 149.27(17) . . ? C16 Cr1 C3 116.63(17) . . ? C13 Cr1 C3 87.70(14) . . ? C14 Cr1 C3 113.23(15) . . ? C5 Cr1 C3 64.45(16) . . ? C4 Cr1 C3 36.29(17) . . ? C2 Cr1 C3 36.11(17) . . ? C1 Cr1 C3 64.39(15) . . ? C6 Cr1 C3 74.98(14) . . ? C6 C1 C2 120.5(4) . . ? C6 C1 C7 120.6(4) . . ? C2 C1 C7 118.9(4) . . ? C6 C1 Cr1 73.0(2) . . ? C2 C1 Cr1 71.5(2) . . ? C7 C1 Cr1 129.7(3) . . ? C3 C2 C1 118.6(4) . . ? C3 C2 C8 120.0(5) . . ? C1 C2 C8 121.3(5) . . ? C3 C2 Cr1 73.0(2) . . ? C1 C2 Cr1 72.1(2) . . ? C8 C2 Cr1 129.7(3) . . ? C2 C3 C4 120.0(4) . . ? C2 C3 C9 120.6(5) . . ? C4 C3 C9 119.3(5) . . ? C2 C3 Cr1 70.9(2) . . ? C4 C3 Cr1 70.2(2) . . ? C9 C3 Cr1 135.2(3) . . ? C5 C4 C3 119.9(4) . . ? C5 C4 C10 120.1(5) . . ? C3 C4 C10 119.9(5) . . ? C5 C4 Cr1 71.9(2) . . ? C3 C4 Cr1 73.5(2) . . ? C10 C4 Cr1 125.1(3) . . ? C4 C5 C6 119.7(4) . . ? C4 C5 C11 121.5(4) . . ? C6 C5 C11 118.6(4) . . ? C4 C5 Cr1 72.4(2) . . ? C6 C5 Cr1 73.4(2) . . ? C11 C5 Cr1 130.2(3) . . ? C1 C6 C5 121.0(4) . . ? C1 C6 C12 118.9(5) . . ? C5 C6 C12 120.1(5) . . ? C1 C6 Cr1 72.1(2) . . ? C5 C6 Cr1 70.3(2) . . ? C12 C6 Cr1 130.5(3) . . ? C14 C13 C21 142.6(4) . . ? C14 C13 Cr1 74.2(2) . . ? C21 C13 Cr1 143.1(3) . . ? C13 C14 C27 144.6(4) . . ? C13 C14 Cr1 69.8(2) . . ? C27 C14 Cr1 143.0(3) . . ? O1 C15 Cr1 174.4(3) . . ? N1 C16 Cr1 176.3(3) . . ? C16 N1 C35 163.7(4) . . ? C26 C21 C22 118.5(3) . . ? C26 C21 C13 121.9(3) . . ? C22 C21 C13 119.5(3) . . ? C23 C22 C21 120.8(4) . . ? C24 C23 C22 119.8(4) . . ? O2 C24 C23 124.3(4) . . ? O2 C24 C25 115.8(4) . . ? C23 C24 C25 120.0(4) . . ? C26 C25 C24 120.1(4) . . ? C25 C26 C21 120.8(4) . . ? C24 O2 C33 117.5(3) . . ? C28 C27 C32 117.3(3) . . ? C28 C27 C14 119.6(3) . . ? C32 C27 C14 123.0(3) . . ? C29 C28 C27 122.4(3) . . ? C28 C29 C30 118.8(3) . . ? O3 C30 C31 115.4(3) . . ? O3 C30 C29 124.8(3) . . ? C31 C30 C29 119.8(3) . . ? C32 C31 C30 120.6(4) . . ? C31 C32 C27 121.0(3) . . ? C30 O3 C34 117.9(3) . . ? C36 C35 C40 123.8(4) . . ? C36 C35 N1 118.8(4) . . ? C40 C35 N1 117.4(3) . . ? C35 C36 C37 116.6(4) . . ? C35 C36 C41 121.1(4) . . ? C37 C36 C41 122.2(4) . . ? C38 C37 C36 120.8(4) . . ? C39 C38 C37 120.6(4) . . ? C38 C39 C40 120.6(4) . . ? C39 C40 C35 117.2(4) . . ? C39 C40 C42 121.6(4) . . ? C35 C40 C42 121.1(4) . . ? F6' P1 F2 111.1(7) . . ? F6' P1 F3' 95.8(6) . . ? F2 P1 F3' 151.2(8) . . ? F6' P1 F5 138.6(7) . . ? F2 P1 F5 95.2(5) . . ? F3' P1 F5 56.5(7) . . ? F6' P1 F1' 92.6(6) . . ? F2 P1 F1' 73.5(7) . . ? F3' P1 F1' 96.0(9) . . ? F5 P1 F1' 64.2(6) . . ? F6' P1 F4' 93.6(6) . . ? F2 P1 F4' 97.2(10) . . ? F3' P1 F4' 90.9(11) . . ? F5 P1 F4' 114.9(6) . . ? F1' P1 F4' 170.3(9) . . ? F6' P1 F4 115.2(7) . . ? F2 P1 F4 96.7(8) . . ? F3' P1 F4 80.1(7) . . ? F5 P1 F4 91.7(4) . . ? F1' P1 F4 152.2(6) . . ? F4' P1 F4 23.5(6) . . ? F6' P1 F1 58.6(6) . . ? F2 P1 F1 92.1(7) . . ? F3' P1 F1 93.4(5) . . ? F5 P1 F1 90.2(4) . . ? F1' P1 F1 34.4(5) . . ? F4' P1 F1 152.1(6) . . ? F4 P1 F1 170.8(7) . . ? F6' P1 F6 35.7(7) . . ? F2 P1 F6 92.2(5) . . ? F3' P1 F6 116.2(9) . . ? F5 P1 F6 172.4(5) . . ? F1' P1 F6 116.9(6) . . ? F4' P1 F6 65.5(6) . . ? F4 P1 F6 88.9(5) . . ? F1 P1 F6 88.1(4) . . ? F6' P1 F2' 89.5(6) . . ? F2 P1 F2' 26.5(6) . . ? F3' P1 F2' 172.5(7) . . ? F5 P1 F2' 121.7(5) . . ? F1' P1 F2' 89.0(8) . . ? F4' P1 F2' 83.5(10) . . ? F4 P1 F2' 92.8(8) . . ? F1 P1 F2' 93.9(6) . . ? F6 P1 F2' 65.8(6) . . ? F6' P1 F5' 173.9(6) . . ? F2 P1 F5' 63.4(6) . . ? F3' P1 F5' 90.0(6) . . ? F5 P1 F5' 46.9(4) . . ? F1' P1 F5' 88.5(5) . . ? F4' P1 F5' 84.7(5) . . ? F4 P1 F5' 64.2(6) . . ? F1 P1 F5' 122.8(5) . . ? F6 P1 F5' 139.2(5) . . ? F2' P1 F5' 84.5(5) . . ? F6' P1 F3 65.9(6) . . ? F2 P1 F3 176.5(7) . . ? F3' P1 F3 31.1(7) . . ? F5 P1 F3 86.4(4) . . ? F1' P1 F3 104.6(7) . . ? F4' P1 F3 84.8(8) . . ? F4 P1 F3 86.3(7) . . ? F1 P1 F3 84.8(5) . . ? F6 P1 F3 86.1(4) . . ? F2' P1 F3 151.9(5) . . ? F5' P1 F3 119.6(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.495 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.067 #===END