# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Ekkehardt Hahn' _publ_contact_author_address ; Institut fur Anorganische und Analytische Chemie Westfalische Wilhelms Universitat Muenster Corrensstrasse 36 Munster D-48149 GERMANY ; _publ_contact_author_email FEHAHN@UNI-MUENSTER.DE _publ_section_title ; Template controlled synthesis of a coordinated [11]ane-P2CNHC macrocycle ; loop_ _publ_author_name 'Ekkehardt Hahn' 'Peter G. Edwards' 'Oliver Kaufhold' 'Andreas Stasch' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 624140' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H20 F4 P2' _chemical_formula_weight 518.40 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' 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' _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 10.966(2) _cell_length_b 14.272(3) _cell_length_c 15.942(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.88(3) _cell_angle_gamma 90.00 _cell_volume 2493.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.222 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8965 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4630 _reflns_number_gt 3481 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0376P)^2^+1.2816P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4630 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 P1 P -0.04524(5) 0.52571(4) 0.29161(4) 0.02524(16) Uani 1 1 d . . . F1 F -0.20163(14) 0.37366(11) 0.23260(10) 0.0539(5) Uani 1 1 d . . . C1 C 0.0769(2) 0.44072(16) 0.31727(13) 0.0245(5) Uani 1 1 d . . . P2 P 0.19974(5) 0.54245(4) 0.19608(4) 0.02574(16) Uani 1 1 d . . . F2 F -0.17670(14) 0.70252(11) 0.31023(11) 0.0555(5) Uani 1 1 d . . . C2 C 0.1868(2) 0.44869(16) 0.27488(14) 0.0262(5) Uani 1 1 d . . . F3 F 0.21168(13) 0.61041(10) 0.02189(8) 0.0404(4) Uani 1 1 d . . . C3 C 0.2805(2) 0.38441(17) 0.29193(15) 0.0329(6) Uani 1 1 d . . . H3 H 0.3555 0.3902 0.2642 0.040 Uiso 1 1 calc R . . F4 F 0.35395(14) 0.64563(13) 0.31910(10) 0.0588(5) Uani 1 1 d . . . C4 C 0.2651(2) 0.31230(18) 0.34881(16) 0.0362(6) Uani 1 1 d . . . H4 H 0.3292 0.2688 0.3598 0.043 Uiso 1 1 calc R . . C5 C 0.1565(2) 0.30396(18) 0.38945(16) 0.0359(6) Uani 1 1 d . . . H5 H 0.1455 0.2543 0.4281 0.043 Uiso 1 1 calc R . . C6 C 0.0635(2) 0.36764(17) 0.37405(14) 0.0311(6) Uani 1 1 d . . . H6 H -0.0108 0.3614 0.4027 0.037 Uiso 1 1 calc R . . C7 C -0.1777(2) 0.47843(16) 0.34587(14) 0.0268(5) Uani 1 1 d . . . C8 C -0.2449(2) 0.40855(19) 0.30551(15) 0.0373(6) Uani 1 1 d . . . C9 C -0.3533(2) 0.3739(2) 0.33381(17) 0.0430(7) Uani 1 1 d . . . H9 H -0.3963 0.3260 0.3039 0.052 Uiso 1 1 calc R . . C10 C -0.3975(2) 0.4104(2) 0.40626(18) 0.0447(7) Uani 1 1 d . . . H10 H -0.4724 0.3880 0.4269 0.054 Uiso 1 1 calc R . . C11 C -0.3336(2) 0.4797(2) 0.44960(17) 0.0417(7) Uani 1 1 d . . . H11 H -0.3643 0.5044 0.5001 0.050 Uiso 1 1 calc R . . C12 C -0.2244(2) 0.51316(18) 0.41922(15) 0.0328(6) Uani 1 1 d . . . H12 H -0.1810 0.5607 0.4494 0.039 Uiso 1 1 calc R . . C13 C -0.0012(2) 0.62347(16) 0.36090(14) 0.0266(5) Uani 1 1 d . . . C14 C -0.0716(2) 0.70337(18) 0.35936(16) 0.0368(6) Uani 1 1 d . . . C15 C -0.0442(3) 0.78315(19) 0.40406(18) 0.0478(7) Uani 1 1 d . . . H15 H -0.0960 0.8365 0.4008 0.057 Uiso 1 1 calc R . . C16 C 0.0611(3) 0.7832(2) 0.45388(17) 0.0472(7) Uani 1 1 d . . . H16 H 0.0828 0.8375 0.4855 0.057 Uiso 1 1 calc R . . C17 C 0.1345(2) 0.70561(18) 0.45796(15) 0.0368(6) Uani 1 1 d . . . H17 H 0.2067 0.7063 0.4926 0.044 Uiso 1 1 calc R . . C18 C 0.1044(2) 0.62614(17) 0.41201(14) 0.0296(5) Uani 1 1 d . . . H18 H 0.1562 0.5728 0.4153 0.035 Uiso 1 1 calc R . . C19 C 0.16880(19) 0.47457(17) 0.09982(14) 0.0274(5) Uani 1 1 d . . . C20 C 0.1726(2) 0.51951(18) 0.02250(15) 0.0310(6) Uani 1 1 d . . . C21 C 0.1392(2) 0.4789(2) -0.05261(15) 0.0353(6) Uani 1 1 d . . . H21 H 0.1439 0.5127 -0.1037 0.042 Uiso 1 1 calc R . . C22 C 0.0984(2) 0.3872(2) -0.05184(16) 0.0404(7) Uani 1 1 d . . . H22 H 0.0744 0.3572 -0.1030 0.049 Uiso 1 1 calc R . . C23 C 0.0924(2) 0.33941(19) 0.02277(16) 0.0392(6) Uani 1 1 d . . . H23 H 0.0640 0.2765 0.0228 0.047 Uiso 1 1 calc R . . C24 C 0.1273(2) 0.38181(18) 0.09802(15) 0.0328(6) Uani 1 1 d . . . H24 H 0.1230 0.3475 0.1489 0.039 Uiso 1 1 calc R . . C25 C 0.3655(2) 0.55893(16) 0.19416(14) 0.0265(5) Uani 1 1 d . . . C26 C 0.4226(2) 0.61301(19) 0.25577(15) 0.0357(6) Uani 1 1 d . . . C27 C 0.5449(2) 0.6351(2) 0.25783(17) 0.0438(7) Uani 1 1 d . . . H27 H 0.5796 0.6725 0.3018 0.053 Uiso 1 1 calc R . . C28 C 0.6159(2) 0.6017(2) 0.19463(16) 0.0394(7) Uani 1 1 d . . . H28 H 0.7004 0.6164 0.1942 0.047 Uiso 1 1 calc R . . C29 C 0.5635(2) 0.54660(19) 0.13187(16) 0.0367(6) Uani 1 1 d . . . H29 H 0.6124 0.5229 0.0886 0.044 Uiso 1 1 calc R . . C30 C 0.4404(2) 0.52584(18) 0.13163(15) 0.0320(6) Uani 1 1 d . . . H30 H 0.4060 0.4881 0.0878 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0228(3) 0.0248(3) 0.0280(3) 0.0006(3) 0.0007(2) -0.0008(3) F1 0.0572(10) 0.0525(11) 0.0530(9) -0.0238(8) 0.0161(8) -0.0262(8) C1 0.0264(12) 0.0215(12) 0.0256(11) -0.0041(10) -0.0005(9) -0.0023(10) P2 0.0224(3) 0.0255(3) 0.0295(3) 0.0016(3) 0.0041(2) -0.0001(3) F2 0.0456(9) 0.0368(9) 0.0828(12) 0.0000(8) -0.0193(9) 0.0119(7) C2 0.0257(12) 0.0249(13) 0.0282(12) -0.0022(10) 0.0021(10) -0.0016(10) F3 0.0388(8) 0.0439(9) 0.0384(8) 0.0095(7) -0.0005(6) -0.0130(7) C3 0.0274(13) 0.0302(14) 0.0414(14) 0.0018(12) 0.0036(11) 0.0023(11) F4 0.0416(9) 0.0826(13) 0.0529(10) -0.0304(9) 0.0113(8) -0.0136(9) C4 0.0340(14) 0.0294(14) 0.0450(15) 0.0034(12) -0.0002(12) 0.0091(11) C5 0.0433(15) 0.0276(14) 0.0369(14) 0.0077(12) 0.0014(12) 0.0003(12) C6 0.0347(14) 0.0270(14) 0.0318(13) 0.0047(11) 0.0057(11) -0.0023(11) C7 0.0223(12) 0.0270(13) 0.0309(12) 0.0025(11) -0.0008(10) 0.0034(10) C8 0.0367(15) 0.0389(16) 0.0365(14) -0.0030(12) 0.0049(12) -0.0061(12) C9 0.0324(14) 0.0437(17) 0.0529(17) 0.0009(14) 0.0014(13) -0.0135(12) C10 0.0266(14) 0.0501(18) 0.0578(18) 0.0123(15) 0.0089(13) -0.0029(13) C11 0.0349(15) 0.0479(17) 0.0430(15) 0.0042(14) 0.0119(12) 0.0052(13) C12 0.0293(13) 0.0341(15) 0.0351(13) 0.0002(11) 0.0016(11) 0.0011(11) C13 0.0275(12) 0.0235(13) 0.0291(12) 0.0029(10) 0.0045(10) -0.0026(10) C14 0.0347(14) 0.0276(15) 0.0479(15) 0.0019(12) -0.0034(12) 0.0011(11) C15 0.0562(18) 0.0247(15) 0.0628(19) -0.0018(14) 0.0073(15) 0.0057(13) C16 0.066(2) 0.0318(16) 0.0442(16) -0.0094(13) 0.0080(15) -0.0160(15) C17 0.0397(15) 0.0376(16) 0.0333(13) -0.0028(12) 0.0021(11) -0.0138(13) C18 0.0287(13) 0.0306(14) 0.0295(12) 0.0013(11) 0.0018(10) -0.0026(11) C19 0.0186(11) 0.0309(14) 0.0328(12) -0.0010(11) 0.0015(10) 0.0032(10) C20 0.0190(11) 0.0370(15) 0.0373(14) 0.0018(12) 0.0044(10) 0.0017(11) C21 0.0219(12) 0.0539(18) 0.0301(13) -0.0005(13) 0.0024(10) 0.0050(12) C22 0.0276(13) 0.0519(18) 0.0417(15) -0.0197(14) -0.0008(11) 0.0069(13) C23 0.0367(15) 0.0301(15) 0.0504(16) -0.0099(13) -0.0031(12) 0.0037(12) C24 0.0298(13) 0.0311(14) 0.0374(14) -0.0009(12) 0.0008(11) 0.0034(11) C25 0.0253(12) 0.0247(13) 0.0295(12) 0.0044(10) 0.0016(10) -0.0014(10) C26 0.0303(13) 0.0443(16) 0.0328(13) -0.0035(12) 0.0072(11) -0.0008(12) C27 0.0339(15) 0.0527(18) 0.0444(15) -0.0080(14) -0.0036(12) -0.0107(13) C28 0.0234(13) 0.0489(17) 0.0458(15) 0.0091(13) 0.0008(12) -0.0053(12) C29 0.0259(13) 0.0466(17) 0.0380(14) 0.0067(13) 0.0064(11) 0.0059(12) C30 0.0252(12) 0.0338(14) 0.0370(13) 0.0010(12) 0.0007(10) 0.0008(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 P1 C13 1.835(2) . ? P1 C1 1.843(2) . ? P1 C7 1.843(2) . ? F1 C8 1.364(3) . ? C1 C6 1.392(3) . ? C1 C2 1.406(3) . ? P2 C25 1.834(2) . ? P2 C19 1.837(2) . ? P2 C2 1.844(2) . ? F2 C14 1.372(3) . ? C2 C3 1.398(3) . ? F3 C20 1.367(3) . ? C3 C4 1.386(3) . ? F4 C26 1.362(3) . ? C4 C5 1.380(3) . ? C5 C6 1.382(3) . ? C7 C12 1.383(3) . ? C7 C8 1.386(3) . ? C8 C9 1.378(3) . ? C9 C10 1.370(4) . ? C10 C11 1.384(4) . ? C11 C12 1.391(3) . ? C13 C14 1.377(3) . ? C13 C18 1.394(3) . ? C14 C15 1.371(4) . ? C15 C16 1.380(4) . ? C16 C17 1.370(4) . ? C17 C18 1.384(3) . ? C19 C20 1.391(3) . ? C19 C24 1.400(3) . ? C20 C21 1.370(3) . ? C21 C22 1.383(4) . ? C22 C23 1.374(4) . ? C23 C24 1.386(3) . ? C25 C26 1.383(3) . ? C25 C30 1.395(3) . ? C26 C27 1.377(3) . ? C27 C28 1.378(4) . ? C28 C29 1.383(4) . ? C29 C30 1.382(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 C13 P1 C1 101.05(10) . . ? C13 P1 C7 101.07(10) . . ? C1 P1 C7 103.48(10) . . ? C6 C1 C2 118.9(2) . . ? C6 C1 P1 123.10(17) . . ? C2 C1 P1 117.92(17) . . ? C25 P2 C19 102.11(10) . . ? C25 P2 C2 101.71(10) . . ? C19 P2 C2 99.80(11) . . ? C3 C2 C1 119.3(2) . . ? C3 C2 P2 122.42(17) . . ? C1 C2 P2 118.22(17) . . ? C4 C3 C2 120.7(2) . . ? C5 C4 C3 119.8(2) . . ? C4 C5 C6 120.2(2) . . ? C5 C6 C1 121.0(2) . . ? C12 C7 C8 116.4(2) . . ? C12 C7 P1 125.77(19) . . ? C8 C7 P1 117.44(17) . . ? F1 C8 C9 118.4(2) . . ? F1 C8 C7 117.6(2) . . ? C9 C8 C7 123.9(2) . . ? C10 C9 C8 118.2(3) . . ? C9 C10 C11 120.4(2) . . ? C10 C11 C12 119.9(2) . . ? C7 C12 C11 121.2(2) . . ? C14 C13 C18 116.3(2) . . ? C14 C13 P1 118.83(18) . . ? C18 C13 P1 124.76(18) . . ? C15 C14 F2 118.0(2) . . ? C15 C14 C13 124.4(2) . . ? F2 C14 C13 117.6(2) . . ? C14 C15 C16 117.7(3) . . ? C17 C16 C15 120.4(3) . . ? C16 C17 C18 120.5(3) . . ? C17 C18 C13 120.7(2) . . ? C20 C19 C24 115.9(2) . . ? C20 C19 P2 119.14(19) . . ? C24 C19 P2 124.53(18) . . ? F3 C20 C21 118.1(2) . . ? F3 C20 C19 117.5(2) . . ? C21 C20 C19 124.4(2) . . ? C20 C21 C22 118.1(2) . . ? C23 C22 C21 120.1(2) . . ? C22 C23 C24 120.9(3) . . ? C23 C24 C19 120.7(2) . . ? C26 C25 C30 115.6(2) . . ? C26 C25 P2 119.07(17) . . ? C30 C25 P2 125.15(18) . . ? F4 C26 C27 117.8(2) . . ? F4 C26 C25 117.9(2) . . ? C27 C26 C25 124.3(2) . . ? C26 C27 C28 118.4(2) . . ? C27 C28 C29 119.6(2) . . ? C30 C29 C28 120.5(2) . . ? C29 C30 C25 121.6(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.518 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.051 #end of data set 3 #complex 5 #start of data set 5 data_complex[5] _database_code_depnum_ccdc_archive 'CCDC 624141' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H6 Cl N2 O4 Re' _chemical_formula_weight 403.79 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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 8.8522(18) _cell_length_b 10.297(2) _cell_length_c 12.389(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.84(3) _cell_angle_gamma 90.00 _cell_volume 1075.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 11.547 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.245 _exptl_absorpt_correction_T_max 0.411 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3540 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 26.99 _reflns_number_total 2315 _reflns_number_gt 2070 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0206P)^2^+3.4853P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2315 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0619 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Re1 Re 0.76977(2) 0.168157(19) 0.146964(15) 0.01686(8) Uani 1 1 d . . . Cl1 Cl 0.90702(14) 0.25526(13) 0.34019(10) 0.0234(3) Uani 1 1 d . . . O1 O 0.4498(5) 0.1939(4) 0.2034(4) 0.0371(10) Uani 1 1 d . . . N1 N 0.7593(5) 0.4194(4) 0.0003(3) 0.0255(10) Uani 1 1 d . . . H1 H 0.7770 0.3708 -0.0530 0.031 Uiso 1 1 calc R . . C1 C 0.7488(5) 0.3714(5) 0.0967(4) 0.0169(9) Uani 1 1 d . . . O2 O 0.7979(5) -0.1136(4) 0.2433(4) 0.0375(10) Uani 1 1 d . . . N2 N 0.7131(6) 0.4669(4) 0.1549(4) 0.0297(11) Uani 1 1 d . . . H2 H 0.6968 0.4557 0.2209 0.036 Uiso 1 1 calc R . . C2 C 0.7389(7) 0.5604(5) -0.0101(4) 0.0265(11) Uani 1 1 d . . . H2A H 0.6497 0.5843 -0.0777 0.032 Uiso 1 1 calc R . . H2B H 0.8369 0.6038 -0.0139 0.032 Uiso 1 1 calc R . . O3 O 1.0968(4) 0.1321(4) 0.1002(3) 0.0315(9) Uani 1 1 d . . . C3 C 0.7028(6) 0.5941(5) 0.0995(4) 0.0253(11) Uani 1 1 d . . . H3A H 0.7821 0.6555 0.1464 0.030 Uiso 1 1 calc R . . H3B H 0.5954 0.6321 0.0836 0.030 Uiso 1 1 calc R . . O4 O 0.5956(5) 0.0801(4) -0.0956(3) 0.0371(10) Uani 1 1 d . . . C4 C 0.5653(6) 0.1847(5) 0.1822(4) 0.0215(11) Uani 1 1 d . . . C5 C 0.7891(6) -0.0115(6) 0.2061(4) 0.0260(11) Uani 1 1 d . . . C6 C 0.9795(6) 0.1502(5) 0.1169(4) 0.0216(11) Uani 1 1 d . . . C7 C 0.6619(6) 0.1120(5) -0.0045(5) 0.0259(11) 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 Re1 0.01759(12) 0.01410(13) 0.01882(13) -0.00013(7) 0.00545(8) -0.00125(7) Cl1 0.0258(6) 0.0274(7) 0.0162(6) 0.0014(5) 0.0052(5) -0.0025(5) O1 0.027(2) 0.035(2) 0.054(3) -0.004(2) 0.020(2) -0.0030(18) N1 0.041(2) 0.018(2) 0.020(2) 0.0008(18) 0.0128(19) 0.005(2) C1 0.015(2) 0.016(2) 0.016(2) -0.0015(19) 0.0001(17) 0.0003(19) O2 0.055(3) 0.019(2) 0.048(3) 0.0099(19) 0.030(2) 0.0057(19) N2 0.054(3) 0.012(2) 0.026(2) -0.0008(18) 0.018(2) 0.006(2) C2 0.036(3) 0.018(3) 0.024(3) 0.005(2) 0.008(2) -0.001(2) O3 0.0218(19) 0.042(2) 0.031(2) -0.0004(19) 0.0080(16) 0.0014(18) C3 0.034(3) 0.011(2) 0.029(3) -0.001(2) 0.006(2) -0.001(2) O4 0.040(2) 0.043(3) 0.023(2) -0.0105(18) 0.0008(17) -0.016(2) C4 0.020(2) 0.021(3) 0.022(3) 0.002(2) 0.005(2) -0.001(2) C5 0.030(3) 0.027(3) 0.028(3) -0.004(2) 0.018(2) 0.002(2) C6 0.025(3) 0.020(3) 0.018(2) 0.001(2) 0.004(2) 0.003(2) C7 0.026(3) 0.024(3) 0.029(3) 0.004(2) 0.010(2) -0.001(2) _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 Re1 C7 1.915(5) . ? Re1 C5 1.978(6) . ? Re1 C4 1.995(5) . ? Re1 C6 2.011(5) . ? Re1 C1 2.175(5) . ? Re1 Cl1 2.4960(14) . ? O1 C4 1.135(6) . ? N1 C1 1.321(6) . ? N1 C2 1.464(7) . ? C1 N2 1.314(6) . ? O2 C5 1.141(7) . ? N2 C3 1.469(6) . ? C2 C3 1.526(7) . ? O3 C6 1.135(6) . ? O4 C7 1.150(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Re1 C5 92.4(2) . . ? C7 Re1 C4 91.5(2) . . ? C5 Re1 C4 88.9(2) . . ? C7 Re1 C6 90.1(2) . . ? C5 Re1 C6 90.1(2) . . ? C4 Re1 C6 178.09(18) . . ? C7 Re1 C1 92.1(2) . . ? C5 Re1 C1 174.95(18) . . ? C4 Re1 C1 88.67(19) . . ? C6 Re1 C1 92.19(19) . . ? C7 Re1 Cl1 176.50(17) . . ? C5 Re1 Cl1 91.10(16) . . ? C4 Re1 Cl1 88.12(15) . . ? C6 Re1 Cl1 90.27(15) . . ? C1 Re1 Cl1 84.42(13) . . ? C1 N1 C2 114.2(4) . . ? N2 C1 N1 108.2(4) . . ? N2 C1 Re1 125.2(4) . . ? N1 C1 Re1 126.5(4) . . ? C1 N2 C3 113.7(4) . . ? N1 C2 C3 101.6(4) . . ? N2 C3 C2 102.3(4) . . ? O1 C4 Re1 179.3(5) . . ? O2 C5 Re1 177.5(4) . . ? O3 C6 Re1 175.9(5) . . ? O4 C7 Re1 178.9(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.941 _refine_diff_density_min -2.071 _refine_diff_density_rms 0.179 # Attachment 'complex[4]Clx3THF.cif' data_complex[4]Clx3THF _database_code_depnum_ccdc_archive 'CCDC 624142' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H50 Cl F4 N2 O6 P2 Re' _chemical_formula_weight 1110.49 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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 11.201(5) _cell_length_b 11.800(5) _cell_length_c 20.504(5) _cell_angle_alpha 92.239(5) _cell_angle_beta 100.058(5) _cell_angle_gamma 117.123(5) _cell_volume 2353.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 2.773 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.3378 _exptl_absorpt_correction_T_max 0.4901 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16641 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9177 _reflns_number_gt 8650 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Two of the three THF molecules are disordered, one of them was refined isotropically with two positions for each atom, one was refined isotropically with two positions for one carbon atom and two positions for the oxigen atom. This THF molecule is refined without hydrogen atoms. The last one was refined anisotropically. ; _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^)+(0.0365P)^2^+8.1029P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9177 _refine_ls_number_parameters 551 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.094 _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 Re1 Re 0.538888(18) 0.377193(17) 0.226789(9) 0.02311(7) Uani 1 1 d . . . Cl1 Cl 0.81939(14) 0.60156(13) 0.09273(7) 0.0401(3) Uani 1 1 d . . . P1 P 0.32000(12) 0.36061(12) 0.23909(6) 0.0250(3) Uani 1 1 d . . . P2 P 0.42437(13) 0.15639(11) 0.24798(6) 0.0259(3) Uani 1 1 d . . . F1 F 0.0903(3) 0.4271(4) 0.25588(16) 0.0468(8) Uani 1 1 d . . . F2 F 0.4795(3) 0.6226(3) 0.31345(17) 0.0445(8) Uani 1 1 d . . . F3 F 0.6824(4) 0.2078(4) 0.34083(18) 0.0521(9) Uani 1 1 d . . . F4 F 0.3591(4) -0.1176(3) 0.28170(18) 0.0553(10) Uani 1 1 d . . . N1 N 0.3370(4) 0.2210(4) 0.0866(2) 0.0331(10) Uani 1 1 d . . . H1 H 0.2769 0.1655 0.1070 0.040 Uiso 1 1 calc R . . N2 N 0.5296(5) 0.3714(4) 0.0734(2) 0.0356(10) Uani 1 1 d . . . H2 H 0.6119 0.4385 0.0832 0.043 Uiso 1 1 calc R . . O1 O 0.6574(4) 0.6653(3) 0.2067(2) 0.0454(10) Uani 1 1 d . . . O2 O 0.6617(4) 0.4764(4) 0.37801(18) 0.0415(9) Uani 1 1 d . . . O3 O 0.8038(4) 0.3612(4) 0.2150(2) 0.0433(9) Uani 1 1 d . . . C1 C 0.4599(5) 0.3154(5) 0.1192(2) 0.0274(10) Uani 1 1 d . . . C2 C 0.3126(6) 0.2195(6) 0.0134(3) 0.0459(14) Uani 1 1 d . . . H2A H 0.2468 0.2520 -0.0025 0.055 Uiso 1 1 calc R . . H2B H 0.2787 0.1323 -0.0104 0.055 Uiso 1 1 calc R . . C3 C 0.4564(7) 0.3107(6) 0.0051(3) 0.0480(15) Uani 1 1 d . . . H3A H 0.4988 0.2633 -0.0139 0.058 Uiso 1 1 calc R . . H3B H 0.4551 0.3752 -0.0241 0.058 Uiso 1 1 calc R . . C4 C 0.6145(5) 0.5587(5) 0.2118(2) 0.0293(10) Uani 1 1 d . . . C5 C 0.6146(5) 0.4381(5) 0.3220(3) 0.0296(10) Uani 1 1 d . . . C6 C 0.7079(5) 0.3692(5) 0.2181(2) 0.0313(11) Uani 1 1 d . . . C7 C 0.2443(5) 0.4432(5) 0.1863(2) 0.0300(10) Uani 1 1 d . . . C8 C 0.1392(5) 0.4660(5) 0.2000(3) 0.0342(11) Uani 1 1 d . . . C9 C 0.0805(6) 0.5253(6) 0.1600(3) 0.0431(14) Uani 1 1 d . . . H9 H 0.0105 0.5409 0.1718 0.052 Uiso 1 1 calc R . . C10 C 0.1256(7) 0.5620(6) 0.1019(3) 0.0493(15) Uani 1 1 d . . . H10 H 0.0845 0.6012 0.0727 0.059 Uiso 1 1 calc R . . C11 C 0.2299(6) 0.5420(6) 0.0861(3) 0.0439(14) Uani 1 1 d . . . H11 H 0.2610 0.5683 0.0463 0.053 Uiso 1 1 calc R . . C12 C 0.2895(5) 0.4838(5) 0.1281(3) 0.0336(11) Uani 1 1 d . . . H12 H 0.3620 0.4714 0.1170 0.040 Uiso 1 1 calc R . . C13 C 0.3189(5) 0.4122(5) 0.3243(2) 0.0289(10) Uani 1 1 d . . . C14 C 0.4048(5) 0.5384(5) 0.3519(3) 0.0331(11) Uani 1 1 d . . . C15 C 0.4190(7) 0.5851(7) 0.4169(3) 0.0498(15) Uani 1 1 d . . . H15 H 0.4794 0.6728 0.4341 0.060 Uiso 1 1 calc R . . C16 C 0.3433(8) 0.5013(7) 0.4562(3) 0.0571(18) Uani 1 1 d . . . H16 H 0.3520 0.5312 0.5014 0.069 Uiso 1 1 calc R . . C17 C 0.2548(7) 0.3742(7) 0.4310(3) 0.0525(17) Uani 1 1 d . . . H17 H 0.2026 0.3171 0.4587 0.063 Uiso 1 1 calc R . . C18 C 0.2422(6) 0.3297(6) 0.3648(3) 0.0375(12) Uani 1 1 d . . . H18 H 0.1806 0.2424 0.3473 0.045 Uiso 1 1 calc R . . C19 C 0.1919(5) 0.1896(5) 0.2224(2) 0.0289(10) Uani 1 1 d . . . C20 C 0.2383(5) 0.0972(5) 0.2228(2) 0.0296(10) Uani 1 1 d . . . C21 C 0.1445(6) -0.0324(5) 0.2059(3) 0.0383(12) Uani 1 1 d . . . H21 H 0.1765 -0.0944 0.2062 0.046 Uiso 1 1 calc R . . C22 C 0.0042(6) -0.0723(6) 0.1885(3) 0.0468(15) Uani 1 1 d . . . H22 H -0.0595 -0.1608 0.1755 0.056 Uiso 1 1 calc R . . C23 C -0.0415(6) 0.0182(6) 0.1905(3) 0.0502(16) Uani 1 1 d . . . H23 H -0.1374 -0.0094 0.1808 0.060 Uiso 1 1 calc R . . C24 C 0.0493(5) 0.1482(5) 0.2064(3) 0.0397(13) Uani 1 1 d . . . H24 H 0.0159 0.2091 0.2065 0.048 Uiso 1 1 calc R . . C25 C 0.4485(6) 0.1390(5) 0.3369(3) 0.0322(11) Uani 1 1 d . . . C26 C 0.5780(6) 0.1712(5) 0.3738(3) 0.0404(13) Uani 1 1 d . . . C27 C 0.6063(8) 0.1675(6) 0.4418(3) 0.0527(17) Uani 1 1 d . . . H27 H 0.6966 0.1898 0.4653 0.063 Uiso 1 1 calc R . . C28 C 0.4994(9) 0.1305(6) 0.4744(3) 0.0552(18) Uani 1 1 d . . . H28 H 0.5169 0.1282 0.5212 0.066 Uiso 1 1 calc R . . C29 C 0.3677(8) 0.0966(6) 0.4406(3) 0.0525(17) Uani 1 1 d . . . H29 H 0.2950 0.0710 0.4638 0.063 Uiso 1 1 calc R . . C30 C 0.3427(7) 0.1005(5) 0.3717(3) 0.0411(13) Uani 1 1 d . . . H30 H 0.2519 0.0765 0.3481 0.049 Uiso 1 1 calc R . . C31 C 0.4626(5) 0.0361(5) 0.2107(3) 0.0316(11) Uani 1 1 d . . . C32 C 0.4313(6) -0.0818(5) 0.2324(3) 0.0392(13) Uani 1 1 d . . . C33 C 0.4672(7) -0.1696(5) 0.2066(3) 0.0442(14) Uani 1 1 d . . . H33 H 0.4431 -0.2496 0.2231 0.053 Uiso 1 1 calc R . . C34 C 0.5393(7) -0.1363(6) 0.1562(3) 0.0456(14) Uani 1 1 d . . . H34 H 0.5664 -0.1938 0.1379 0.055 Uiso 1 1 calc R . . C35 C 0.5719(6) -0.0214(6) 0.1323(3) 0.0424(13) Uani 1 1 d . . . H35 H 0.6202 -0.0004 0.0971 0.051 Uiso 1 1 calc R . . C36 C 0.5346(5) 0.0648(5) 0.1594(3) 0.0340(11) Uani 1 1 d . . . H36 H 0.5586 0.1445 0.1426 0.041 Uiso 1 1 calc R . . O4 O 0.8788(6) 0.2455(5) 0.5596(3) 0.0776(16) Uani 1 1 d . . . C37 C 0.9691(11) 0.3702(11) 0.5508(6) 0.113(4) Uani 1 1 d . . . H37A H 0.9263 0.3971 0.5123 0.136 Uiso 1 1 calc R . . H37B H 1.0544 0.3734 0.5417 0.136 Uiso 1 1 calc R . . C38 C 1.0023(10) 0.4594(10) 0.6138(6) 0.100(3) Uani 1 1 d . . . H38A H 1.0968 0.5317 0.6219 0.120 Uiso 1 1 calc R . . H38B H 0.9361 0.4937 0.6125 0.120 Uiso 1 1 calc R . . C39 C 0.9873(12) 0.3689(10) 0.6645(5) 0.102(3) Uani 1 1 d . . . H39A H 0.9733 0.4002 0.7066 0.122 Uiso 1 1 calc R . . H39B H 1.0669 0.3518 0.6743 0.122 Uiso 1 1 calc R . . C40 C 0.8602(12) 0.2540(10) 0.6265(6) 0.104(3) Uani 1 1 d . . . H40A H 0.8489 0.1753 0.6462 0.125 Uiso 1 1 calc R . . H40B H 0.7780 0.2649 0.6274 0.125 Uiso 1 1 calc R . . O5 O 1.0081(11) 1.0598(11) 0.4078(8) 0.068(4) Uiso 0.457(16) 1 d PD A 1 C41 C 0.8934(13) 1.0867(15) 0.3899(11) 0.062(5) Uiso 0.457(16) 1 d PD A 1 H41A H 0.9126 1.1512 0.3584 0.075 Uiso 0.457(16) 1 calc PR A 1 H41B H 0.8755 1.1199 0.4302 0.075 Uiso 0.457(16) 1 calc PR A 1 C42 C 0.773(2) 0.9610(17) 0.3575(15) 0.107(9) Uiso 0.457(16) 1 d PD A 1 H42A H 0.6882 0.9514 0.3711 0.128 Uiso 0.457(16) 1 calc PR A 1 H42B H 0.7577 0.9553 0.3082 0.128 Uiso 0.457(16) 1 calc PR A 1 C43 C 0.808(2) 0.859(2) 0.3815(15) 0.104(11) Uiso 0.457(16) 1 d PD A 1 H43A H 0.8151 0.8093 0.3438 0.125 Uiso 0.457(16) 1 calc PR A 1 H43B H 0.7384 0.8000 0.4045 0.125 Uiso 0.457(16) 1 calc PR A 1 C44 C 0.945(2) 0.9338(16) 0.4291(14) 0.135(11) Uiso 0.457(16) 1 d PD A 1 H44C H 0.9325 0.9409 0.4755 0.162 Uiso 0.457(16) 1 calc PR A 1 H44D H 1.0024 0.8909 0.4272 0.162 Uiso 0.457(16) 1 calc PR A 1 O5A O 0.9951(11) 1.0440(9) 0.3729(8) 0.078(4) Uiso 0.543(16) 1 d PD A 2 C41A C 0.8737(14) 1.0615(18) 0.3576(12) 0.091(6) Uiso 0.543(16) 1 d PD A 2 H41C H 0.8442 1.0553 0.3086 0.109 Uiso 0.543(16) 1 calc PR A 2 H41D H 0.8949 1.1477 0.3780 0.109 Uiso 0.543(16) 1 calc PR A 2 C42A C 0.7603(15) 0.9601(14) 0.3842(10) 0.078(5) Uiso 0.543(16) 1 d PD A 2 H42C H 0.7433 0.9977 0.4234 0.094 Uiso 0.543(16) 1 calc PR A 2 H42D H 0.6742 0.9180 0.3495 0.094 Uiso 0.543(16) 1 calc PR A 2 C43A C 0.8111(14) 0.8660(16) 0.4038(10) 0.072(6) Uiso 0.543(16) 1 d PD A 2 H43C H 0.7414 0.7771 0.3844 0.086 Uiso 0.543(16) 1 calc PR A 2 H43D H 0.8338 0.8706 0.4531 0.086 Uiso 0.543(16) 1 calc PR A 2 C44A C 0.9373(13) 0.9070(9) 0.3757(8) 0.064(4) Uiso 0.543(16) 1 d PD A 2 H44A H 1.0049 0.8881 0.4045 0.077 Uiso 0.543(16) 1 calc PR A 2 H44B H 0.9132 0.8601 0.3303 0.077 Uiso 0.543(16) 1 calc PR A 2 C48 C 0.2738(9) 0.8386(10) 0.9861(4) 0.1024(15) Uiso 1 1 d D . . C45 C 0.2360(9) 0.8870(11) 1.0437(5) 0.1024(15) Uiso 1 1 d D B . C46 C 0.0908(9) 0.8646(10) 1.0238(5) 0.1024(15) Uiso 1 1 d D . . C47 C 0.0457(13) 0.7666(16) 0.9637(8) 0.1024(15) Uiso 0.586(9) 1 d PD B 1 C47A C 0.0393(16) 0.839(3) 0.9494(5) 0.1024(15) Uiso 0.414(9) 1 d PD B 2 O6 O 0.1484(9) 0.7379(10) 0.9441(6) 0.1024(15) Uiso 0.586(9) 1 d PD B 1 O6A O 0.1659(14) 0.8447(18) 0.9381(7) 0.1024(15) Uiso 0.414(9) 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02103(11) 0.02434(11) 0.02300(11) 0.00287(7) 0.00342(7) 0.01036(8) Cl1 0.0330(7) 0.0416(7) 0.0442(8) 0.0096(6) 0.0080(6) 0.0160(6) P1 0.0224(6) 0.0281(6) 0.0248(6) 0.0055(5) 0.0053(5) 0.0121(5) P2 0.0255(6) 0.0235(6) 0.0264(6) 0.0023(5) 0.0054(5) 0.0098(5) F1 0.0438(19) 0.075(2) 0.0423(19) 0.0240(17) 0.0198(15) 0.0407(19) F2 0.0465(19) 0.0313(16) 0.0471(19) 0.0009(14) 0.0158(15) 0.0095(15) F3 0.0402(19) 0.062(2) 0.054(2) 0.0154(18) 0.0019(16) 0.0259(18) F4 0.087(3) 0.0383(19) 0.051(2) 0.0178(16) 0.030(2) 0.032(2) N1 0.031(2) 0.033(2) 0.027(2) 0.0048(17) 0.0017(18) 0.0099(19) N2 0.033(2) 0.043(3) 0.023(2) 0.0026(18) 0.0054(18) 0.011(2) O1 0.047(2) 0.024(2) 0.066(3) 0.0092(18) 0.021(2) 0.0148(18) O2 0.041(2) 0.052(2) 0.026(2) -0.0026(17) -0.0007(16) 0.0196(19) O3 0.0248(19) 0.053(2) 0.058(3) 0.009(2) 0.0117(17) 0.0228(19) C1 0.028(2) 0.028(2) 0.028(2) 0.0062(19) 0.006(2) 0.015(2) C2 0.048(4) 0.054(4) 0.025(3) 0.003(2) -0.004(2) 0.019(3) C3 0.052(4) 0.058(4) 0.023(3) 0.002(2) 0.004(2) 0.018(3) C4 0.023(2) 0.036(3) 0.030(3) 0.002(2) 0.008(2) 0.013(2) C5 0.023(2) 0.030(3) 0.034(3) 0.006(2) 0.008(2) 0.011(2) C6 0.032(3) 0.028(2) 0.029(3) 0.007(2) 0.005(2) 0.010(2) C7 0.028(3) 0.033(3) 0.030(3) 0.005(2) 0.005(2) 0.015(2) C8 0.029(3) 0.045(3) 0.035(3) 0.013(2) 0.013(2) 0.020(2) C9 0.038(3) 0.058(4) 0.049(3) 0.020(3) 0.014(3) 0.033(3) C10 0.048(4) 0.066(4) 0.052(4) 0.032(3) 0.016(3) 0.038(3) C11 0.044(3) 0.059(4) 0.042(3) 0.027(3) 0.019(3) 0.031(3) C12 0.033(3) 0.037(3) 0.035(3) 0.011(2) 0.011(2) 0.018(2) C13 0.030(3) 0.035(3) 0.027(2) 0.007(2) 0.006(2) 0.020(2) C14 0.032(3) 0.039(3) 0.034(3) 0.002(2) 0.010(2) 0.020(2) C15 0.059(4) 0.053(4) 0.038(3) -0.006(3) 0.005(3) 0.029(3) C16 0.077(5) 0.076(5) 0.034(3) 0.005(3) 0.011(3) 0.049(4) C17 0.069(4) 0.074(5) 0.038(3) 0.026(3) 0.030(3) 0.047(4) C18 0.039(3) 0.044(3) 0.040(3) 0.012(2) 0.016(2) 0.026(3) C19 0.028(3) 0.030(2) 0.025(2) 0.0024(19) 0.0052(19) 0.011(2) C20 0.028(3) 0.030(2) 0.026(2) 0.0032(19) 0.005(2) 0.010(2) C21 0.036(3) 0.029(3) 0.041(3) 0.004(2) 0.009(2) 0.007(2) C22 0.034(3) 0.034(3) 0.053(4) -0.003(3) 0.006(3) 0.001(3) C23 0.022(3) 0.054(4) 0.060(4) 0.004(3) 0.006(3) 0.007(3) C24 0.027(3) 0.040(3) 0.048(3) 0.005(2) 0.005(2) 0.013(2) C25 0.044(3) 0.025(2) 0.031(3) 0.007(2) 0.006(2) 0.019(2) C26 0.048(3) 0.032(3) 0.041(3) 0.009(2) 0.001(3) 0.021(3) C27 0.069(4) 0.039(3) 0.046(4) 0.002(3) -0.010(3) 0.029(3) C28 0.103(6) 0.042(3) 0.029(3) 0.007(3) 0.010(3) 0.041(4) C29 0.084(5) 0.049(4) 0.038(3) 0.017(3) 0.026(3) 0.038(4) C30 0.054(4) 0.037(3) 0.036(3) 0.012(2) 0.015(3) 0.022(3) C31 0.034(3) 0.030(3) 0.032(3) 0.003(2) 0.003(2) 0.017(2) C32 0.049(3) 0.034(3) 0.033(3) 0.004(2) 0.007(2) 0.018(3) C33 0.062(4) 0.033(3) 0.041(3) 0.002(2) 0.004(3) 0.027(3) C34 0.056(4) 0.040(3) 0.047(3) -0.004(3) 0.005(3) 0.030(3) C35 0.043(3) 0.043(3) 0.045(3) 0.000(3) 0.013(3) 0.023(3) C36 0.033(3) 0.033(3) 0.035(3) 0.002(2) 0.005(2) 0.016(2) O4 0.076(4) 0.068(4) 0.061(3) 0.007(3) -0.007(3) 0.018(3) C37 0.081(7) 0.103(8) 0.099(8) 0.031(7) 0.014(6) -0.004(6) C38 0.072(6) 0.075(6) 0.139(10) -0.006(6) -0.009(6) 0.036(5) C39 0.133(10) 0.082(7) 0.080(7) -0.017(5) 0.008(6) 0.050(7) C40 0.106(8) 0.088(7) 0.110(8) 0.020(6) 0.056(7) 0.027(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 Re1 C5 1.950(5) . ? Re1 C4 1.971(5) . ? Re1 C6 1.975(6) . ? Re1 C1 2.188(5) . ? Re1 P2 2.4204(16) . ? Re1 P1 2.4280(16) . ? P1 C13 1.831(5) . ? P1 C7 1.833(5) . ? P1 C19 1.839(5) . ? P2 C25 1.829(5) . ? P2 C20 1.835(5) . ? P2 C31 1.835(5) . ? F1 C8 1.362(6) . ? F2 C14 1.358(6) . ? F3 C26 1.360(7) . ? F4 C32 1.365(7) . ? N1 C1 1.343(6) . ? N1 C2 1.477(7) . ? N2 C1 1.328(6) . ? N2 C3 1.459(7) . ? O1 C4 1.141(6) . ? O2 C5 1.154(6) . ? O3 C6 1.132(6) . ? C2 C3 1.520(9) . ? C7 C8 1.392(7) . ? C7 C12 1.394(7) . ? C8 C9 1.367(7) . ? C9 C10 1.383(8) . ? C10 C11 1.379(8) . ? C11 C12 1.387(7) . ? C13 C14 1.379(7) . ? C13 C18 1.388(7) . ? C14 C15 1.376(8) . ? C15 C16 1.371(10) . ? C16 C17 1.380(10) . ? C17 C18 1.397(8) . ? C19 C20 1.405(7) . ? C19 C24 1.411(7) . ? C20 C21 1.389(7) . ? C21 C22 1.392(8) . ? C22 C23 1.380(9) . ? C23 C24 1.384(8) . ? C25 C26 1.383(8) . ? C25 C30 1.396(8) . ? C26 C27 1.381(8) . ? C27 C28 1.377(10) . ? C28 C29 1.378(10) . ? C29 C30 1.399(8) . ? C31 C32 1.384(7) . ? C31 C36 1.396(8) . ? C32 C33 1.386(8) . ? C33 C34 1.382(9) . ? C34 C35 1.369(8) . ? C35 C36 1.393(7) . ? O4 C37 1.396(11) . ? O4 C40 1.430(11) . ? C37 C38 1.511(15) . ? C38 C39 1.495(14) . ? C39 C40 1.497(14) . ? O5 C41 1.4499(12) . ? O5 C44 1.4499(12) . ? C41 C42 1.5002(12) . ? C42 C43 1.5000(11) . ? C43 C44 1.5001(12) . ? O5A C44A 1.4496(12) . ? O5A C41A 1.4499(12) . ? C41A C42A 1.5001(11) . ? C42A C43A 1.5001(11) . ? C43A C44A 1.5002(12) . ? C48 O6 1.4494(11) . ? C48 O6A 1.4508(11) . ? C48 C45 1.4994(11) . ? C45 C46 1.4999(13) . ? C46 C47A 1.4997(11) . ? C46 C47 1.5004(11) . ? C47 O6 1.4505(11) . ? C47A O6A 1.4501(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Re1 C4 87.7(2) . . ? C5 Re1 C6 90.0(2) . . ? C4 Re1 C6 93.1(2) . . ? C5 Re1 C1 177.9(2) . . ? C4 Re1 C1 90.45(19) . . ? C6 Re1 C1 89.10(19) . . ? C5 Re1 P2 91.53(15) . . ? C4 Re1 P2 173.60(14) . . ? C6 Re1 P2 93.21(15) . . ? C1 Re1 P2 90.43(13) . . ? C5 Re1 P1 90.50(15) . . ? C4 Re1 P1 93.54(14) . . ? C6 Re1 P1 173.31(14) . . ? C1 Re1 P1 90.60(13) . . ? P2 Re1 P1 80.11(5) . . ? C13 P1 C7 104.4(2) . . ? C13 P1 C19 104.4(2) . . ? C7 P1 C19 105.8(2) . . ? C13 P1 Re1 113.68(16) . . ? C7 P1 Re1 119.40(17) . . ? C19 P1 Re1 107.94(17) . . ? C25 P2 C20 102.7(2) . . ? C25 P2 C31 103.4(2) . . ? C20 P2 C31 107.4(2) . . ? C25 P2 Re1 113.38(16) . . ? C20 P2 Re1 108.19(17) . . ? C31 P2 Re1 120.27(18) . . ? C1 N1 C2 113.5(4) . . ? C1 N2 C3 113.4(5) . . ? N2 C1 N1 107.3(4) . . ? N2 C1 Re1 123.7(4) . . ? N1 C1 Re1 128.9(4) . . ? N1 C2 C3 100.8(4) . . ? N2 C3 C2 103.1(5) . . ? O1 C4 Re1 176.1(4) . . ? O2 C5 Re1 178.5(5) . . ? O3 C6 Re1 177.2(5) . . ? C8 C7 C12 116.7(5) . . ? C8 C7 P1 123.4(4) . . ? C12 C7 P1 119.9(4) . . ? F1 C8 C9 117.4(5) . . ? F1 C8 C7 119.0(4) . . ? C9 C8 C7 123.6(5) . . ? C8 C9 C10 118.3(5) . . ? C11 C10 C9 120.4(5) . . ? C10 C11 C12 120.2(5) . . ? C11 C12 C7 120.8(5) . . ? C14 C13 C18 117.2(5) . . ? C14 C13 P1 118.9(4) . . ? C18 C13 P1 123.8(4) . . ? F2 C14 C15 117.5(5) . . ? F2 C14 C13 118.9(5) . . ? C15 C14 C13 123.6(5) . . ? C16 C15 C14 118.0(6) . . ? C15 C16 C17 120.9(6) . . ? C16 C17 C18 119.7(6) . . ? C13 C18 C17 120.5(6) . . ? C20 C19 C24 119.0(5) . . ? C20 C19 P1 118.6(4) . . ? C24 C19 P1 122.4(4) . . ? C21 C20 C19 120.1(5) . . ? C21 C20 P2 123.0(4) . . ? C19 C20 P2 116.9(4) . . ? C20 C21 C22 120.6(5) . . ? C23 C22 C21 119.2(5) . . ? C22 C23 C24 121.6(5) . . ? C23 C24 C19 119.5(5) . . ? C26 C25 C30 116.7(5) . . ? C26 C25 P2 120.0(4) . . ? C30 C25 P2 123.2(4) . . ? F3 C26 C27 118.7(6) . . ? F3 C26 C25 117.7(5) . . ? C27 C26 C25 123.6(6) . . ? C28 C27 C26 117.9(6) . . ? C27 C28 C29 121.5(6) . . ? C28 C29 C30 119.0(6) . . ? C25 C30 C29 121.3(6) . . ? C32 C31 C36 116.0(5) . . ? C32 C31 P2 124.4(4) . . ? C36 C31 P2 119.6(4) . . ? F4 C32 C31 119.3(5) . . ? F4 C32 C33 116.4(5) . . ? C31 C32 C33 124.3(6) . . ? C34 C33 C32 117.6(5) . . ? C35 C34 C33 120.7(5) . . ? C34 C35 C36 120.3(6) . . ? C35 C36 C31 121.2(5) . . ? C37 O4 C40 105.8(7) . . ? O4 C37 C38 108.7(9) . . ? C39 C38 C37 100.1(8) . . ? C38 C39 C40 98.7(9) . . ? O4 C40 C39 105.8(8) . . ? C41 O5 C44 102.7(15) . . ? O5 C41 C42 105.8(14) . . ? C43 C42 C41 105.5(17) . . ? C42 C43 C44 104.0(19) . . ? O5 C44 C43 105.9(16) . . ? C44A O5A C41A 102.5(11) . . ? O5A C41A C42A 109.6(11) . . ? C43A C42A C41A 104.7(12) . . ? C42A C43A C44A 104.1(12) . . ? O5A C44A C43A 107.7(10) . . ? O6 C48 O6A 48.8(8) . . ? O6 C48 C45 107.8(8) . . ? O6A C48 C45 92.2(9) . . ? C48 C45 C46 109.6(8) . . ? C47A C46 C45 112.3(9) . . ? C47A C46 C47 36.8(11) . . ? C45 C46 C47 97.5(9) . . ? O6 C47 C46 117.7(10) . . ? O6A C47A C46 92.2(11) . . ? C48 O6 C47 101.5(9) . . ? C47A O6A C48 128.0(13) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 4.133 _refine_diff_density_min -1.231 _refine_diff_density_rms 0.119 # Attachment 'complex[5]Clx3H2O.cif' data_complex[5]Clx3H2O _database_code_depnum_ccdc_archive 'CCDC 624143' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 Cl F2 N2 O6 P2 Re' _chemical_formula_weight 908.21 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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 9.030(5) _cell_length_b 10.898(5) _cell_length_c 19.929(5) _cell_angle_alpha 75.388(5) _cell_angle_beta 82.356(5) _cell_angle_gamma 68.013(5) _cell_volume 1758.1(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 3.682 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.4046 _exptl_absorpt_correction_T_max 0.7097 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11366 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7586 _reflns_number_gt 6915 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogen atoms of the H2O molecules where not refined. ; _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^)+(0.0054P)^2^+4.2575P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7586 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.037516(16) 0.212830(15) 0.806615(7) 0.02139(5) Uani 1 1 d . . . Cl1 Cl 0.23214(15) 0.62400(12) 0.53444(7) 0.0463(3) Uani 1 1 d . . . P1 P 0.14574(11) 0.39052(10) 0.77659(5) 0.0220(2) Uani 1 1 d . . . F1 F -0.0987(3) 0.5353(3) 0.87332(15) 0.0489(7) Uani 1 1 d . . . O1 O -0.3076(4) 0.4224(4) 0.8048(2) 0.0559(10) Uani 1 1 d . . . N1 N 0.0098(4) 0.3657(4) 0.64949(16) 0.0295(7) Uani 1 1 d . . . C1 C 0.0641(4) 0.2444(4) 0.69431(19) 0.0238(8) Uani 1 1 d . . . P2 P 0.31244(11) 0.07700(9) 0.79221(5) 0.01933(19) Uani 1 1 d . . . F2 F 0.2422(3) -0.1249(3) 0.91010(13) 0.0435(7) Uani 1 1 d . . . O2 O 0.0320(4) 0.1715(3) 0.96634(15) 0.0425(8) Uani 1 1 d . . . N2 N 0.1358(4) 0.1482(3) 0.65777(16) 0.0272(7) Uani 1 1 d . . . C2 C 0.0504(6) 0.3542(5) 0.5759(2) 0.0431(12) Uani 1 1 d . . . H2A H 0.1269 0.3998 0.5544 0.052 Uiso 1 1 calc R . . H2B H -0.0466 0.3940 0.5484 0.052 Uiso 1 1 calc R . . O3 O -0.0603(4) -0.0344(3) 0.81267(18) 0.0476(8) Uani 1 1 d . . . C3 C 0.1247(6) 0.2035(5) 0.5816(2) 0.0367(10) Uani 1 1 d . . . H3A H 0.0564 0.1701 0.5616 0.044 Uiso 1 1 calc R . . H3B H 0.2318 0.1788 0.5578 0.044 Uiso 1 1 calc R . . O4 O 0.5519(5) 0.0661(4) 0.5387(2) 0.0595(10) Uani 1 1 d . . . C4 C -0.0447(5) 0.4987(4) 0.6629(2) 0.0314(9) Uani 1 1 d . . . O5 O 0.1397(4) 0.9290(4) 0.46802(18) 0.0522(9) Uani 1 1 d . . . C5 C -0.1567(5) 0.6024(5) 0.6192(2) 0.0405(11) Uani 1 1 d . . . H5 H -0.2054 0.5813 0.5864 0.049 Uiso 1 1 calc R . . O6 O 0.5680(4) 0.6482(4) 0.50754(19) 0.0543(9) Uani 1 1 d . . . C6 C -0.1973(6) 0.7354(5) 0.6233(3) 0.0517(14) Uani 1 1 d . . . H6 H -0.2751 0.8053 0.5938 0.062 Uiso 1 1 calc R . . C7 C -0.1255(6) 0.7680(5) 0.6703(3) 0.0487(13) Uani 1 1 d . . . H7 H -0.1492 0.8601 0.6713 0.058 Uiso 1 1 calc R . . C8 C -0.0191(5) 0.6650(4) 0.7155(2) 0.0364(10) Uani 1 1 d . . . H8 H 0.0266 0.6872 0.7490 0.044 Uiso 1 1 calc R . . C9 C 0.0230(4) 0.5288(4) 0.7132(2) 0.0287(9) Uani 1 1 d . . . C10 C 0.1766(5) 0.4689(4) 0.8411(2) 0.0258(8) Uani 1 1 d . . . C11 C 0.0490(5) 0.5326(4) 0.8830(2) 0.0333(9) Uani 1 1 d . . . C12 C 0.0641(6) 0.5936(4) 0.9327(2) 0.0417(11) Uani 1 1 d . . . H12 H -0.0265 0.6378 0.9594 0.050 Uiso 1 1 calc R . . C13 C 0.2147(6) 0.5893(5) 0.9430(2) 0.0427(12) Uani 1 1 d . . . H13 H 0.2281 0.6298 0.9777 0.051 Uiso 1 1 calc R . . C14 C 0.3440(6) 0.5275(4) 0.9039(2) 0.0376(10) Uani 1 1 d . . . H14 H 0.4467 0.5255 0.9113 0.045 Uiso 1 1 calc R . . C15 C 0.3261(5) 0.4676(4) 0.8532(2) 0.0306(9) Uani 1 1 d . . . H15 H 0.4172 0.4249 0.8263 0.037 Uiso 1 1 calc R . . C16 C 0.3412(4) 0.3265(4) 0.73328(19) 0.0223(8) Uani 1 1 d . . . C17 C 0.4175(4) 0.1861(4) 0.74114(18) 0.0208(7) Uani 1 1 d . . . C18 C 0.5626(5) 0.1349(4) 0.7057(2) 0.0270(8) Uani 1 1 d . . . H18 H 0.6132 0.0397 0.7100 0.032 Uiso 1 1 calc R . . C19 C 0.6337(5) 0.2221(4) 0.6641(2) 0.0308(9) Uani 1 1 d . . . H19 H 0.7347 0.1866 0.6412 0.037 Uiso 1 1 calc R . . C20 C 0.5573(5) 0.3610(4) 0.6558(2) 0.0310(9) Uani 1 1 d . . . H20 H 0.6053 0.4208 0.6267 0.037 Uiso 1 1 calc R . . C21 C 0.4113(5) 0.4132(4) 0.6898(2) 0.0272(8) Uani 1 1 d . . . H21 H 0.3589 0.5086 0.6835 0.033 Uiso 1 1 calc R . . C22 C 0.4341(4) -0.0230(4) 0.86632(19) 0.0229(8) Uani 1 1 d . . . C23 C 0.3825(5) -0.1125(4) 0.9182(2) 0.0287(9) Uani 1 1 d . . . C24 C 0.4655(6) -0.1885(5) 0.9763(2) 0.0388(10) Uani 1 1 d . . . H24 H 0.4249 -0.2476 1.0105 0.047 Uiso 1 1 calc R . . C25 C 0.6104(6) -0.1777(5) 0.9845(2) 0.0425(11) Uani 1 1 d . . . H25 H 0.6712 -0.2309 1.0239 0.051 Uiso 1 1 calc R . . C26 C 0.6651(5) -0.0890(5) 0.9348(2) 0.0410(11) Uani 1 1 d . . . H26 H 0.7631 -0.0802 0.9406 0.049 Uiso 1 1 calc R . . C27 C 0.5786(5) -0.0126(4) 0.8765(2) 0.0308(9) Uani 1 1 d . . . H27 H 0.6183 0.0478 0.8428 0.037 Uiso 1 1 calc R . . C28 C 0.3275(5) -0.0397(4) 0.73878(19) 0.0250(8) Uani 1 1 d . . . C29 C 0.2282(5) 0.0089(4) 0.6814(2) 0.0279(9) Uani 1 1 d . . . C30 C 0.2307(6) -0.0803(5) 0.6420(2) 0.0382(11) Uani 1 1 d . . . H30 H 0.1630 -0.0491 0.6039 0.046 Uiso 1 1 calc R . . C31 C 0.3316(7) -0.2145(5) 0.6580(2) 0.0451(12) Uani 1 1 d . . . H31 H 0.3330 -0.2745 0.6304 0.054 Uiso 1 1 calc R . . C32 C 0.4306(6) -0.2626(5) 0.7136(2) 0.0419(11) Uani 1 1 d . . . H32 H 0.5005 -0.3546 0.7238 0.050 Uiso 1 1 calc R . . C33 C 0.4263(5) -0.1744(4) 0.7542(2) 0.0310(9) Uani 1 1 d . . . H33 H 0.4920 -0.2071 0.7930 0.037 Uiso 1 1 calc R . . C34 C -0.1825(5) 0.3444(5) 0.8046(2) 0.0355(10) Uani 1 1 d . . . C35 C 0.0342(4) 0.1857(4) 0.9073(2) 0.0286(9) Uani 1 1 d . . . C36 C -0.0278(5) 0.0576(5) 0.8118(2) 0.0316(9) 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 Re1 0.01662(8) 0.02547(9) 0.01994(9) -0.00009(6) -0.00202(6) -0.00785(6) Cl1 0.0451(6) 0.0454(7) 0.0500(7) -0.0099(6) -0.0048(5) -0.0176(5) P1 0.0180(4) 0.0196(5) 0.0245(5) -0.0024(4) -0.0006(4) -0.0041(4) F1 0.0295(13) 0.0537(17) 0.0625(19) -0.0265(15) 0.0134(13) -0.0101(12) O1 0.0199(16) 0.060(2) 0.069(3) -0.0018(19) -0.0036(16) -0.0005(16) N1 0.0290(17) 0.037(2) 0.0210(17) 0.0042(15) -0.0059(14) -0.0150(15) C1 0.0190(17) 0.034(2) 0.0208(19) -0.0005(16) -0.0045(15) -0.0151(16) P2 0.0191(4) 0.0192(5) 0.0191(5) -0.0029(4) -0.0023(4) -0.0065(4) F2 0.0471(16) 0.0434(15) 0.0434(15) 0.0105(12) -0.0136(12) -0.0289(13) O2 0.0426(18) 0.058(2) 0.0228(16) -0.0108(15) -0.0018(14) -0.0115(16) N2 0.0369(19) 0.0336(19) 0.0159(16) 0.0016(14) -0.0068(14) -0.0204(16) C2 0.071(3) 0.048(3) 0.020(2) 0.003(2) -0.012(2) -0.034(3) O3 0.048(2) 0.048(2) 0.059(2) -0.0099(17) 0.0029(17) -0.0332(17) C3 0.042(2) 0.047(3) 0.021(2) 0.0019(19) -0.0063(18) -0.019(2) O4 0.061(2) 0.053(2) 0.072(3) -0.015(2) 0.001(2) -0.0276(19) C4 0.0215(19) 0.034(2) 0.028(2) 0.0055(18) -0.0023(16) -0.0063(17) O5 0.046(2) 0.056(2) 0.054(2) -0.0216(18) -0.0080(17) -0.0080(17) C5 0.026(2) 0.044(3) 0.038(3) 0.011(2) -0.0064(19) -0.008(2) O6 0.052(2) 0.060(2) 0.061(2) -0.0205(19) -0.0068(18) -0.0247(19) C6 0.029(2) 0.043(3) 0.051(3) 0.018(2) -0.004(2) 0.004(2) C7 0.040(3) 0.028(2) 0.053(3) 0.005(2) 0.007(2) 0.005(2) C8 0.035(2) 0.025(2) 0.040(3) -0.0003(19) 0.0013(19) -0.0047(18) C9 0.0216(18) 0.026(2) 0.032(2) 0.0019(17) -0.0003(16) -0.0066(16) C10 0.0258(19) 0.0195(19) 0.028(2) -0.0047(16) 0.0017(16) -0.0048(15) C11 0.031(2) 0.026(2) 0.039(2) -0.0062(19) 0.0043(19) -0.0096(18) C12 0.051(3) 0.033(2) 0.041(3) -0.020(2) 0.020(2) -0.014(2) C13 0.070(3) 0.037(3) 0.032(2) -0.015(2) 0.008(2) -0.030(2) C14 0.048(3) 0.038(3) 0.035(2) -0.011(2) 0.001(2) -0.024(2) C15 0.034(2) 0.025(2) 0.032(2) -0.0047(18) 0.0015(18) -0.0120(18) C16 0.0227(18) 0.0237(19) 0.0191(18) -0.0031(15) -0.0030(15) -0.0071(15) C17 0.0222(17) 0.0261(19) 0.0158(18) -0.0042(15) -0.0035(14) -0.0098(15) C18 0.028(2) 0.027(2) 0.025(2) -0.0078(17) 0.0014(16) -0.0087(17) C19 0.026(2) 0.037(2) 0.029(2) -0.0094(18) 0.0052(17) -0.0124(18) C20 0.031(2) 0.035(2) 0.029(2) -0.0024(18) 0.0026(17) -0.0177(19) C21 0.031(2) 0.022(2) 0.027(2) -0.0023(16) -0.0029(17) -0.0100(17) C22 0.0262(19) 0.0186(18) 0.0222(19) -0.0054(15) -0.0026(15) -0.0048(15) C23 0.030(2) 0.026(2) 0.029(2) -0.0012(17) -0.0049(17) -0.0104(17) C24 0.045(3) 0.034(2) 0.030(2) 0.0072(19) -0.006(2) -0.013(2) C25 0.040(3) 0.044(3) 0.030(2) 0.003(2) -0.012(2) -0.005(2) C26 0.030(2) 0.054(3) 0.035(3) 0.000(2) -0.0131(19) -0.013(2) C27 0.025(2) 0.036(2) 0.028(2) -0.0026(18) -0.0017(17) -0.0098(18) C28 0.031(2) 0.027(2) 0.0222(19) -0.0059(16) 0.0025(16) -0.0168(17) C29 0.039(2) 0.031(2) 0.022(2) -0.0044(17) -0.0007(17) -0.0223(19) C30 0.067(3) 0.037(3) 0.023(2) -0.0017(19) -0.006(2) -0.034(2) C31 0.082(4) 0.037(3) 0.028(2) -0.011(2) 0.001(2) -0.033(3) C32 0.065(3) 0.027(2) 0.037(3) -0.009(2) 0.004(2) -0.021(2) C33 0.038(2) 0.028(2) 0.028(2) -0.0081(18) 0.0020(18) -0.0132(18) C34 0.025(2) 0.044(3) 0.032(2) 0.003(2) -0.0036(18) -0.012(2) C35 0.0213(19) 0.032(2) 0.030(2) -0.0058(18) -0.0018(16) -0.0069(17) C36 0.024(2) 0.044(3) 0.028(2) -0.0034(19) -0.0011(17) -0.0161(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C35 1.950(4) . ? Re1 C36 1.966(4) . ? Re1 C34 1.966(4) . ? Re1 C1 2.172(4) . ? Re1 P2 2.3895(14) . ? Re1 P1 2.3957(13) . ? P1 C9 1.804(4) . ? P1 C10 1.814(4) . ? P1 C16 1.823(4) . ? F1 C11 1.361(5) . ? O1 C34 1.131(5) . ? N1 C1 1.350(5) . ? N1 C4 1.428(5) . ? N1 C2 1.488(5) . ? C1 N2 1.342(5) . ? P2 C28 1.813(4) . ? P2 C22 1.817(4) . ? P2 C17 1.824(4) . ? F2 C23 1.357(5) . ? O2 C35 1.147(5) . ? N2 C29 1.420(5) . ? N2 C3 1.487(5) . ? C2 C3 1.504(7) . ? O3 C36 1.141(5) . ? C4 C5 1.392(6) . ? C4 C9 1.402(6) . ? C5 C6 1.376(7) . ? C6 C7 1.387(8) . ? C7 C8 1.381(6) . ? C8 C9 1.399(6) . ? C10 C11 1.394(5) . ? C10 C15 1.397(6) . ? C11 C12 1.370(6) . ? C12 C13 1.384(7) . ? C13 C14 1.364(6) . ? C14 C15 1.388(6) . ? C16 C21 1.391(5) . ? C16 C17 1.399(5) . ? C17 C18 1.390(5) . ? C18 C19 1.386(5) . ? C19 C20 1.385(6) . ? C20 C21 1.384(6) . ? C22 C23 1.393(5) . ? C22 C27 1.396(5) . ? C23 C24 1.368(6) . ? C24 C25 1.391(6) . ? C25 C26 1.379(6) . ? C26 C27 1.386(6) . ? C28 C33 1.381(6) . ? C28 C29 1.415(5) . ? C29 C30 1.388(5) . ? C30 C31 1.384(7) . ? C31 C32 1.386(7) . ? C32 C33 1.392(6) . ? 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 C35 Re1 C36 93.19(17) . . ? C35 Re1 C34 90.63(17) . . ? C36 Re1 C34 94.23(18) . . ? C35 Re1 C1 174.40(14) . . ? C36 Re1 C1 90.52(15) . . ? C34 Re1 C1 93.27(16) . . ? C35 Re1 P2 96.60(11) . . ? C36 Re1 P2 91.15(13) . . ? C34 Re1 P2 170.73(13) . . ? C1 Re1 P2 79.12(10) . . ? C35 Re1 P1 97.93(12) . . ? C36 Re1 P1 167.33(12) . . ? C34 Re1 P1 91.72(13) . . ? C1 Re1 P1 77.96(10) . . ? P2 Re1 P1 81.58(5) . . ? C9 P1 C10 105.29(19) . . ? C9 P1 C16 106.01(18) . . ? C10 P1 C16 105.18(17) . . ? C9 P1 Re1 109.15(13) . . ? C10 P1 Re1 122.21(13) . . ? C16 P1 Re1 107.93(13) . . ? C1 N1 C4 129.0(3) . . ? C1 N1 C2 112.2(4) . . ? C4 N1 C2 117.1(3) . . ? N2 C1 N1 108.6(3) . . ? N2 C1 Re1 126.3(3) . . ? N1 C1 Re1 125.1(3) . . ? C28 P2 C22 106.33(18) . . ? C28 P2 C17 104.65(17) . . ? C22 P2 C17 105.65(17) . . ? C28 P2 Re1 108.88(13) . . ? C22 P2 Re1 121.51(13) . . ? C17 P2 Re1 108.58(13) . . ? C1 N2 C29 129.3(3) . . ? C1 N2 C3 112.5(3) . . ? C29 N2 C3 118.0(3) . . ? N1 C2 C3 103.1(3) . . ? N2 C3 C2 103.1(3) . . ? C5 C4 C9 120.0(4) . . ? C5 C4 N1 117.8(4) . . ? C9 C4 N1 121.9(3) . . ? C6 C5 C4 120.4(5) . . ? C5 C6 C7 120.4(4) . . ? C8 C7 C6 119.2(5) . . ? C7 C8 C9 121.6(5) . . ? C8 C9 C4 118.1(4) . . ? C8 C9 P1 122.9(3) . . ? C4 C9 P1 118.7(3) . . ? C11 C10 C15 116.1(4) . . ? C11 C10 P1 120.6(3) . . ? C15 C10 P1 123.3(3) . . ? F1 C11 C12 118.4(4) . . ? F1 C11 C10 118.0(4) . . ? C12 C11 C10 123.6(4) . . ? C11 C12 C13 118.3(4) . . ? C14 C13 C12 120.6(4) . . ? C13 C14 C15 120.3(4) . . ? C14 C15 C10 121.2(4) . . ? C21 C16 C17 119.5(3) . . ? C21 C16 P1 121.8(3) . . ? C17 C16 P1 118.6(3) . . ? C18 C17 C16 119.7(3) . . ? C18 C17 P2 122.1(3) . . ? C16 C17 P2 117.9(3) . . ? C19 C18 C17 120.3(4) . . ? C20 C19 C18 119.9(4) . . ? C21 C20 C19 120.3(4) . . ? C20 C21 C16 120.2(4) . . ? C23 C22 C27 116.2(4) . . ? C23 C22 P2 120.3(3) . . ? C27 C22 P2 123.4(3) . . ? F2 C23 C24 118.5(4) . . ? F2 C23 C22 117.8(3) . . ? C24 C23 C22 123.7(4) . . ? C23 C24 C25 118.8(4) . . ? C26 C25 C24 119.4(4) . . ? C25 C26 C27 120.7(4) . . ? C26 C27 C22 121.1(4) . . ? C33 C28 C29 119.7(4) . . ? C33 C28 P2 122.2(3) . . ? C29 C28 P2 118.0(3) . . ? C30 C29 C28 119.2(4) . . ? C30 C29 N2 117.4(4) . . ? C28 C29 N2 123.1(3) . . ? C31 C30 C29 120.2(4) . . ? C30 C31 C32 121.0(4) . . ? C31 C32 C33 119.1(4) . . ? C28 C33 C32 120.8(4) . . ? O1 C34 Re1 177.6(4) . . ? O2 C35 Re1 179.1(4) . . ? O3 C36 Re1 176.9(4) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.787 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.117