data_Nataro_Ryann_JES _audit_creation_date 2024-10-04 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _shelx_SHELXL_version_number '2019/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C31 H28 Fe O4 P, B F4, 1[CH2Cl2]' _chemical_formula_sum 'C32 H30 B Cl2 F4 Fe O4 P' _chemical_formula_weight 723.09 _chemical_melting_point ? _chemical_oxdiff_formula C31H28BF4FeO4P 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'tetragonal' _space_group_IT_number 88 _space_group_name_H-M_alt 'I 41/a' _space_group_name_Hall '-I 4ad' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 35.6005(7) _cell_length_b 35.6005(7) _cell_length_c 10.5456(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13365.4(6) _cell_formula_units_Z 16 _cell_measurement_reflns_used 14638 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 25.1420 _cell_measurement_theta_min 2.0230 _shelx_estimated_absorpt_T_max 0.952 _shelx_estimated_absorpt_T_min 0.890 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_correction_T_min 0.996 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.124a (Rigaku Oxford Diffraction, 2024) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 5920 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 42 -28 0 0.0493 15 -5 -14 0.0727 1 -6 15 0.0869 -3 -25 13 0.0822 -5 -38 10 0.0765 -2 0 -15 0.0726 -44 23 -1 0.0148 7 2 -15 0.0717 18 47 0 0.0413 -36 -35 0 0.0312 47 17 1 0.0426 27 -42 -1 0.0426 -18 -47 -1 0.0295 _exptl_crystal_size_max 0.167 _exptl_crystal_size_mid 0.077 _exptl_crystal_size_min 0.069 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 41.9680 -27.6020 -0.1390 0.9923 -0.1043 -0.0665 15.4613 -4.9825 -14.0647 0.3809 -0.0400 0.9237 0.6834 -5.9128 14.7600 0.0000 -0.0000 -1.0000 -2.5671 -25.0400 12.8604 0.1994 0.3453 -0.9171 -4.9922 -38.0260 9.5870 0.3427 0.5935 -0.7282 -1.5835 0.3198 -14.8569 0.0565 0.0978 0.9936 -44.4596 23.2730 -0.6603 -0.9722 0.2066 0.1104 7.4963 1.6502 -14.6894 0.1789 -0.0380 0.9831 17.9282 46.8471 -0.2112 -0.3068 -0.9443 0.1191 -35.5247 -35.3968 -0.3141 -0.1044 0.9931 -0.0526 46.9153 17.4800 1.0025 0.4996 -0.8654 -0.0384 27.2143 -42.0751 -1.0087 0.9504 0.3088 -0.0384 -18.0730 -46.7301 -0.7373 0.3085 0.9496 -0.0555 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1653 _diffrn_reflns_av_unetI/netI 0.0881 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 126394 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 24.246 _diffrn_reflns_theta_max 24.246 _diffrn_reflns_theta_min 2.317 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -74.00 110.00 0.50 100.00 -- 20.00 54.00-154.21 368 2 \w -74.00 110.00 0.50 100.00 -- 20.00 54.00-154.21 368 3 \w -74.00 110.00 0.50 100.00 -- 20.00 54.00 -32.11 368 4 \w 22.00 108.00 0.50 100.00 -- 20.00 54.00 90.00 172 5 \w 22.00 108.00 0.50 100.00 -- 20.00 54.00 90.00 172 6 \w -72.00 25.00 0.50 100.00 -- 20.00 54.00 -87.14 194 7 \w 31.00 57.00 0.50 100.00 -- 20.00 54.00 -87.14 52 8 \w -73.00 86.00 0.50 100.00 -- 20.00 54.00 30.00 318 9 \w -71.00 -45.00 0.50 100.00 -- 20.00 54.00 150.00 52 10 \w -13.00 13.00 0.50 100.00 -- 20.00 54.00 150.00 52 11 \w 44.00 93.00 0.50 100.00 -- 20.00 54.00 150.00 98 12 \w -73.00 12.00 0.50 100.00 -- 20.00 54.00-180.00 170 13 \w 42.00 96.00 0.50 100.00 -- 20.00 54.00-180.00 108 14 \w -66.00 -32.00 0.50 100.00 -- 20.00 54.00-120.00 68 15 \w 1.00 27.00 0.50 100.00 -- 20.00 54.00-120.00 52 16 \w -74.00 58.00 0.50 100.00 -- 20.00 54.00 120.00 264 17 \w -73.00 -23.00 0.50 100.00 -- 20.00 54.00 -48.83 100 18 \w -73.00 -27.00 0.50 100.00 -- 20.00 54.00-154.21 92 ; _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini II' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0154202000 _diffrn_orient_matrix_UB_12 -0.0124763000 _diffrn_orient_matrix_UB_13 -0.0057120000 _diffrn_orient_matrix_UB_21 -0.0126045000 _diffrn_orient_matrix_UB_22 -0.0153581000 _diffrn_orient_matrix_UB_23 -0.0055688000 _diffrn_orient_matrix_UB_31 -0.0002650000 _diffrn_orient_matrix_UB_32 0.0023435000 _diffrn_orient_matrix_UB_33 -0.0667998000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3162 _reflns_number_total 5393 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)' _computing_data_collection 'CrysAlisPro system (CCD 43.124a (release 23-05-2024))' _computing_data_reduction 'CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.385 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.071 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 410 _refine_ls_number_reflns 5393 _refine_ls_number_restraints 77 _refine_ls_R_factor_all 0.1313 _refine_ls_R_factor_gt 0.0732 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+82.6221P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1424 _refine_ls_wR_factor_ref 0.1694 _refine_special_details ? _olex2_refinement_description ; 1. Others Fixed Uiso: H4(0.049) H5(0.054) H6(0.055) H7(0.047) H9A(0.043) H9B(0.043) H10(0.042) H12(0.046) H14A(0.111) H14B(0.111) H14C(0.111) H15(0.068) H16(0.061) H17(0.053) H19(0.045) H21A(0.077) H21B(0.077) H21C(0.077) H22(0.048) H23(0.051) H24(0.044) H26(0.05) H28A(0.081) H28B(0.081) H28C(0.081) H29(0.051) H30(0.052) H31(0.045) Fixed X: H4(0.613289) H5(0.613094) H6(0.625955) H7(0.639625) H9A(0.700229) H9B(0.713091) H10(0.656734) H12(0.754947) H14A(0.802362) H14B(0.791675) H14C(0.786583) H15(0.722174) H16(0.661563) H17(0.646893) H19(0.720315) H21A(0.78719) H21B(0.752908) H21C(0.79391) H22(0.810211) H23(0.797042) H24(0.745814) H26(0.67428) H28A(0.615683) H28B(0.660528) H28C(0.638962) H29(0.594098) H30(0.59087) H31(0.629192) Fixed Y: H4(0.295374) H5(0.324312) H6(0.289043) H7(0.22478) H9A(0.273452) H9B(0.239097) H10(0.242192) H12(0.325944) H14A(0.362588) H14B(0.402249) H14C(0.364447) H15(0.415418) H16(0.40991) H17(0.362679) H19(0.226256) H21A(0.18139) H21B(0.174771) H21C(0.183787) H22(0.247854) H23(0.311575) H24(0.33334) H26(0.369248) H28A(0.416315) H28B(0.41394) H28C(0.400763) H29(0.343235) H30(0.282351) H31(0.26435) Fixed Z: H4(0.347859) H5(0.150927) H6(-0.034763) H7(-0.02422) H9A(0.18389) H9B(0.272106) H10(0.388655) H12(0.317868) H14A(0.213817) H14B(0.15216) H14C(0.071857) H15(0.109161) H16(0.186062) H17(0.331841) H19(0.475154) H21A(0.507124) H21B(0.602704) H21C(0.656954) H22(0.696603) H23(0.690537) H24(0.574507) H26(0.571401) H28A(0.739182) H28B(0.732416) H28C(0.857914) H29(0.830826) H30(0.751314) H31(0.580356) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.59322(2) 0.25129(2) 0.15491(8) 0.0400(3) Uani 1 1 d . . . . . P1 P 0.68676(4) 0.30016(4) 0.43658(13) 0.0344(4) Uani 1 1 d . . . . . O4 O 0.52452(14) 0.28687(15) 0.2569(5) 0.0785(17) Uani 1 1 d . . . . . O3 O 0.55158(13) 0.22872(12) -0.0756(4) 0.0553(12) Uani 1 1 d . . . . . O2 O 0.59463(13) 0.18017(13) 0.2971(4) 0.0550(12) Uani 1 1 d . . . . . O1 O 0.68070(11) 0.19079(12) 0.1420(3) 0.0450(11) Uani 1 1 d . . . . . C10 C 0.5517(2) 0.27329(19) 0.2183(6) 0.0535(18) Uani 1 1 d . . . . . C9 C 0.56753(17) 0.23711(17) 0.0149(6) 0.0443(16) Uani 1 1 d . . . . . C8 C 0.59290(18) 0.2082(2) 0.2438(5) 0.0446(16) Uani 1 1 d . . . . . C5 C 0.62806(16) 0.28165(16) 0.2818(5) 0.0409(15) Uani 1 1 d . . . . . H4 H 0.613289 0.295374 0.347859 0.049 Uiso 1 1 calc R U . . . C4 C 0.62553(16) 0.29924(17) 0.1589(6) 0.0447(16) Uani 1 1 d . . . . . H5 H 0.613094 0.324312 0.150927 0.054 Uiso 1 1 calc R U . . . C3 C 0.63332(16) 0.27836(18) 0.0493(6) 0.0457(16) Uani 1 1 d . . . . . H6 H 0.625955 0.289043 -0.034763 0.055 Uiso 1 1 calc R U . . . C2 C 0.64305(15) 0.23916(17) 0.0564(5) 0.0389(15) Uani 1 1 d . . . . . H7 H 0.639625 0.224780 -0.024220 0.047 Uiso 1 1 calc R U . . . C1 C 0.67189(16) 0.22404(19) 0.1427(5) 0.0374(15) Uani 1 1 d . . . . . C7 C 0.69114(15) 0.25141(16) 0.2322(5) 0.0359(14) Uani 1 1 d . . . . . H9A H 0.700229 0.273452 0.183890 0.043 Uiso 1 1 calc R U . . . H9B H 0.713091 0.239097 0.272106 0.043 Uiso 1 1 calc R U . . . C6 C 0.66367(15) 0.26428(16) 0.3350(5) 0.0349(14) Uani 1 1 d . . . . . H10 H 0.656734 0.242192 0.388655 0.042 Uiso 1 1 calc R U . . . C17 C 0.69931(15) 0.33970(16) 0.3384(5) 0.0333(14) Uani 1 1 d . . . . . C18 C 0.73617(17) 0.34319(16) 0.2913(5) 0.0387(15) Uani 1 1 d . . . . . H12 H 0.754947 0.325944 0.317868 0.046 Uiso 1 1 calc R U . . . C19 C 0.74538(18) 0.37168(18) 0.2062(5) 0.0483(17) Uani 1 1 d . . . . . C31 C 0.78497(19) 0.3756(2) 0.1567(7) 0.074(2) Uani 1 1 d . . . . . H14A H 0.802362 0.362588 0.213817 0.111 Uiso 1 1 calc R U . . . H14B H 0.791675 0.402249 0.152160 0.111 Uiso 1 1 calc R U . . . H14C H 0.786583 0.364447 0.071857 0.111 Uiso 1 1 calc R U . . . C20 C 0.7166(2) 0.39606(18) 0.1682(6) 0.0565(19) Uani 1 1 d . . . . . H15 H 0.722174 0.415418 0.109161 0.068 Uiso 1 1 calc R U . . . C21 C 0.68043(19) 0.39289(18) 0.2136(6) 0.0507(17) Uani 1 1 d . . . . . H16 H 0.661563 0.409910 0.186062 0.061 Uiso 1 1 calc R U . . . C22 C 0.67171(18) 0.36480(17) 0.2995(5) 0.0442(16) Uani 1 1 d . . . . . H17 H 0.646893 0.362679 0.331841 0.053 Uiso 1 1 calc R U . . . C11 C 0.72830(15) 0.28190(16) 0.5124(5) 0.0323(14) Uani 1 1 d . . . . . C12 C 0.73624(16) 0.24355(18) 0.5178(5) 0.0378(15) Uani 1 1 d . . . . . H19 H 0.720315 0.226256 0.475154 0.045 Uiso 1 1 calc R U . . . C13 C 0.76739(17) 0.23024(16) 0.5852(5) 0.0374(15) Uani 1 1 d . . . . . C29 C 0.77611(18) 0.18896(17) 0.5883(5) 0.0516(17) Uani 1 1 d . . . . . H21A H 0.787190 0.181390 0.507124 0.077 Uiso 1 1 calc R U . . . H21B H 0.752908 0.174771 0.602704 0.077 Uiso 1 1 calc R U . . . H21C H 0.793910 0.183787 0.656954 0.077 Uiso 1 1 calc R U . . . C14 C 0.78922(16) 0.25639(18) 0.6490(5) 0.0403(15) Uani 1 1 d . . . . . H22 H 0.810211 0.247854 0.696603 0.048 Uiso 1 1 calc R U . . . C15 C 0.78151(17) 0.29439(18) 0.6458(5) 0.0428(16) Uani 1 1 d . . . . . H23 H 0.797042 0.311575 0.690537 0.051 Uiso 1 1 calc R U . . . C16 C 0.75118(16) 0.30721(17) 0.5774(5) 0.0370(14) Uani 1 1 d . . . . . H24 H 0.745814 0.333340 0.574507 0.044 Uiso 1 1 calc R U . . . C23 C 0.65499(15) 0.31509(16) 0.5595(5) 0.0334(14) Uani 1 1 d . . . . . C28 C 0.65746(17) 0.35168(17) 0.6085(5) 0.0414(15) Uani 1 1 d . . . . . H26 H 0.674280 0.369248 0.571401 0.050 Uiso 1 1 calc R U . . . C27 C 0.63501(16) 0.36243(18) 0.7125(5) 0.0410(15) Uani 1 1 d . . . . . C30 C 0.63779(18) 0.40182(18) 0.7651(6) 0.0540(18) Uani 1 1 d . . . . . H28A H 0.615683 0.416315 0.739182 0.081 Uiso 1 1 calc R U . . . H28B H 0.660528 0.413940 0.732416 0.081 Uiso 1 1 calc R U . . . H28C H 0.638962 0.400763 0.857914 0.081 Uiso 1 1 calc R U . . . C26 C 0.60999(16) 0.33615(18) 0.7625(5) 0.0424(16) Uani 1 1 d . . . . . H29 H 0.594098 0.343235 0.830826 0.051 Uiso 1 1 calc R U . . . C25 C 0.60781(17) 0.29990(18) 0.7148(5) 0.0436(16) Uani 1 1 d . . . . . H30 H 0.590870 0.282351 0.751314 0.052 Uiso 1 1 calc R U . . . C24 C 0.63051(15) 0.28920(17) 0.6129(5) 0.0372(15) Uani 1 1 d . . . . . H31 H 0.629192 0.264350 0.580356 0.045 Uiso 1 1 calc R U . . . F4 F 0.6239(3) 0.1837(4) 0.7299(10) 0.0638(13) Uani 0.331(5) 1 d D . P A 2 F2 F 0.6248(4) 0.1627(4) 0.5279(10) 0.083(4) Uani 0.331(5) 1 d D . P A 2 F3 F 0.6750(4) 0.1509(3) 0.6579(11) 0.068(3) Uani 0.331(5) 1 d D . P A 2 F1 F 0.6638(4) 0.2073(5) 0.586(3) 0.066(5) Uani 0.331(5) 1 d D . P A 2 B1 B 0.6460(5) 0.1742(6) 0.6274(18) 0.0638(13) Uani 0.331(5) 1 d D . P A 2 F7 F 0.60711(19) 0.1956(2) 0.5663(6) 0.091(2) Uani 0.669(5) 1 d D . P A 1 F5 F 0.6693(3) 0.1986(3) 0.5954(12) 0.097(4) Uani 0.669(5) 1 d D . P A 1 F6 F 0.6350(3) 0.14865(16) 0.6779(6) 0.098(3) Uani 0.669(5) 1 d D . P A 1 F8 F 0.63126(17) 0.20596(18) 0.7606(5) 0.0638(13) Uani 0.669(5) 1 d D . P A 1 B2 B 0.6363(3) 0.1859(3) 0.6470(10) 0.0638(13) Uani 0.669(5) 1 d D . P A 1 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 Fe1 0.0397(6) 0.0481(6) 0.0321(5) -0.0053(4) -0.0029(4) -0.0007(4) P1 0.0361(9) 0.0450(10) 0.0222(7) -0.0041(7) 0.0023(6) 0.0015(8) O4 0.045(3) 0.099(4) 0.092(4) -0.038(3) 0.004(3) 0.011(3) O3 0.068(3) 0.050(3) 0.048(3) 0.006(2) -0.024(2) -0.006(2) O2 0.076(3) 0.060(3) 0.028(2) 0.002(2) -0.002(2) -0.017(3) O1 0.053(3) 0.047(3) 0.035(2) -0.011(2) 0.0012(19) 0.005(2) C10 0.049(5) 0.057(5) 0.055(4) -0.019(3) -0.012(4) -0.005(4) C9 0.042(4) 0.046(4) 0.045(4) 0.004(3) -0.004(3) -0.003(3) C8 0.052(4) 0.056(5) 0.026(3) -0.006(3) -0.003(3) -0.015(4) C5 0.042(4) 0.044(4) 0.036(3) -0.007(3) -0.001(3) 0.005(3) C4 0.043(4) 0.042(4) 0.050(4) 0.001(3) -0.014(3) 0.001(3) C3 0.040(4) 0.061(5) 0.036(3) 0.012(3) -0.010(3) -0.013(3) C2 0.038(4) 0.057(4) 0.022(3) -0.002(3) 0.002(3) -0.009(3) C1 0.042(4) 0.055(4) 0.016(3) -0.005(3) 0.007(3) 0.001(3) C7 0.037(4) 0.050(4) 0.020(3) -0.001(3) 0.002(2) 0.005(3) C6 0.037(3) 0.042(4) 0.026(3) -0.007(3) 0.000(3) -0.002(3) C17 0.034(3) 0.038(4) 0.027(3) -0.002(3) -0.003(3) 0.005(3) C18 0.043(4) 0.046(4) 0.028(3) -0.003(3) 0.001(3) 0.001(3) C19 0.054(4) 0.056(4) 0.034(3) 0.006(3) 0.010(3) -0.005(4) C31 0.067(5) 0.093(6) 0.062(5) 0.030(4) 0.013(4) 0.001(4) C20 0.083(6) 0.044(4) 0.043(4) 0.012(3) 0.002(4) 0.008(4) C21 0.049(4) 0.061(5) 0.042(4) 0.001(3) -0.006(3) 0.012(4) C22 0.052(4) 0.049(4) 0.031(3) -0.006(3) 0.001(3) 0.000(3) C11 0.035(3) 0.044(4) 0.018(3) -0.003(2) 0.006(2) 0.006(3) C12 0.039(4) 0.061(4) 0.014(3) -0.004(3) 0.003(2) 0.002(3) C13 0.052(4) 0.043(4) 0.018(3) 0.002(3) 0.010(3) 0.010(3) C29 0.063(5) 0.065(5) 0.027(3) 0.007(3) 0.005(3) 0.008(4) C14 0.037(4) 0.068(5) 0.016(3) 0.005(3) 0.002(3) 0.002(3) C15 0.053(4) 0.055(4) 0.021(3) 0.001(3) 0.003(3) 0.000(3) C16 0.045(4) 0.047(4) 0.019(3) -0.005(3) 0.004(3) 0.000(3) C23 0.033(3) 0.047(4) 0.020(3) -0.002(3) -0.001(2) 0.001(3) C28 0.047(4) 0.050(4) 0.028(3) -0.006(3) -0.003(3) -0.001(3) C27 0.039(4) 0.055(4) 0.029(3) -0.015(3) -0.007(3) 0.009(3) C30 0.053(4) 0.074(5) 0.035(4) -0.017(3) -0.007(3) 0.006(4) C26 0.035(4) 0.068(5) 0.024(3) -0.007(3) -0.002(3) 0.012(3) C25 0.046(4) 0.063(5) 0.022(3) 0.004(3) 0.008(3) 0.011(3) C24 0.039(4) 0.047(4) 0.026(3) -0.003(3) -0.005(3) 0.007(3) F4 0.079(3) 0.069(3) 0.043(2) -0.001(2) -0.008(2) -0.019(3) F2 0.108(9) 0.083(9) 0.057(6) -0.005(6) -0.035(6) -0.011(7) F3 0.094(7) 0.048(6) 0.063(7) -0.026(5) -0.033(5) -0.013(5) F1 0.029(7) 0.064(6) 0.104(13) 0.019(7) 0.007(6) 0.006(4) B1 0.079(3) 0.069(3) 0.043(2) -0.001(2) -0.008(2) -0.019(3) F7 0.113(5) 0.100(6) 0.060(4) 0.021(4) -0.044(4) -0.038(4) F5 0.093(5) 0.152(10) 0.046(5) -0.003(6) 0.005(4) -0.043(6) F6 0.164(8) 0.058(3) 0.071(4) 0.008(3) -0.033(5) -0.021(4) F8 0.079(3) 0.069(3) 0.043(2) -0.001(2) -0.008(2) -0.019(3) B2 0.079(3) 0.069(3) 0.043(2) -0.001(2) -0.008(2) -0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C10 1.801(8) . ? Fe1 C9 1.809(7) . ? Fe1 C8 1.799(7) . ? Fe1 C5 2.121(6) . ? Fe1 C4 2.059(6) . ? Fe1 C3 2.051(6) . ? Fe1 C2 2.100(6) . ? P1 C6 1.859(5) . ? P1 C17 1.804(6) . ? P1 C11 1.802(6) . ? P1 C23 1.801(5) . ? O4 C10 1.157(7) . ? O3 C9 1.150(7) . ? O2 C8 1.146(7) . ? O1 C1 1.224(7) . ? C5 H4 1.0000 . ? C5 C4 1.442(8) . ? C5 C6 1.518(8) . ? C4 H5 1.0000 . ? C4 C3 1.402(8) . ? C3 H6 1.0000 . ? C3 C2 1.440(8) . ? C2 H7 1.0000 . ? C2 C1 1.474(8) . ? C1 C7 1.520(7) . ? C7 H9A 0.9900 . ? C7 H9B 0.9900 . ? C7 C6 1.530(7) . ? C6 H10 1.0000 . ? C17 C18 1.408(7) . ? C17 C22 1.390(8) . ? C18 H12 0.9500 . ? C18 C19 1.393(8) . ? C19 C31 1.510(9) . ? C19 C20 1.402(8) . ? C31 H14A 0.9800 . ? C31 H14B 0.9800 . ? C31 H14C 0.9800 . ? C20 H15 0.9500 . ? C20 C21 1.377(9) . ? C21 H16 0.9500 . ? C21 C22 1.385(8) . ? C22 H17 0.9500 . ? C11 C12 1.395(8) . ? C11 C16 1.395(7) . ? C12 H19 0.9500 . ? C12 C13 1.400(7) . ? C13 C29 1.502(8) . ? C13 C14 1.387(8) . ? C29 H21A 0.9800 . ? C29 H21B 0.9800 . ? C29 H21C 0.9800 . ? C14 H22 0.9500 . ? C14 C15 1.381(8) . ? C15 H23 0.9500 . ? C15 C16 1.376(8) . ? C16 H24 0.9500 . ? C23 C28 1.404(8) . ? C23 C24 1.388(7) . ? C28 H26 0.9500 . ? C28 C27 1.411(8) . ? C27 C30 1.512(8) . ? C27 C26 1.395(8) . ? C30 H28A 0.9800 . ? C30 H28B 0.9800 . ? C30 H28C 0.9800 . ? C26 H29 0.9500 . ? C26 C25 1.388(8) . ? C25 H30 0.9500 . ? C25 C24 1.397(7) . ? C24 H31 0.9500 . ? F4 B1 1.378(18) . ? F2 B1 1.357(19) . ? F3 B1 1.364(17) . ? F1 B1 1.41(2) . ? F7 B2 1.388(12) . ? F5 B2 1.371(12) . ? F6 B2 1.367(11) . ? F8 B2 1.406(11) . ? 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 C10 Fe1 C9 90.6(3) . . ? C10 Fe1 C5 91.4(2) . . ? C10 Fe1 C4 95.2(3) . . ? C10 Fe1 C3 124.6(3) . . ? C10 Fe1 C2 165.0(3) . . ? C9 Fe1 C5 162.4(2) . . ? C9 Fe1 C4 122.1(3) . . ? C9 Fe1 C3 92.3(3) . . ? C9 Fe1 C2 88.0(2) . . ? C8 Fe1 C10 99.9(3) . . ? C8 Fe1 C9 100.6(3) . . ? C8 Fe1 C5 96.3(2) . . ? C8 Fe1 C4 134.5(2) . . ? C8 Fe1 C3 133.5(3) . . ? C8 Fe1 C2 95.0(3) . . ? C4 Fe1 C5 40.3(2) . . ? C4 Fe1 C2 73.1(2) . . ? C3 Fe1 C5 72.3(2) . . ? C3 Fe1 C4 39.9(2) . . ? C3 Fe1 C2 40.6(2) . . ? C2 Fe1 C5 85.6(2) . . ? C17 P1 C6 108.4(2) . . ? C11 P1 C6 111.8(3) . . ? C11 P1 C17 109.4(3) . . ? C23 P1 C6 109.9(3) . . ? C23 P1 C17 109.8(3) . . ? C23 P1 C11 107.6(2) . . ? O4 C10 Fe1 178.2(6) . . ? O3 C9 Fe1 178.5(6) . . ? O2 C8 Fe1 176.0(6) . . ? Fe1 C5 H4 112.4 . . ? C4 C5 Fe1 67.5(3) . . ? C4 C5 H4 112.4 . . ? C4 C5 C6 124.1(5) . . ? C6 C5 Fe1 120.9(4) . . ? C6 C5 H4 112.4 . . ? Fe1 C4 H5 119.4 . . ? C5 C4 Fe1 72.2(3) . . ? C5 C4 H5 119.4 . . ? C3 C4 Fe1 69.8(3) . . ? C3 C4 C5 119.9(6) . . ? C3 C4 H5 119.4 . . ? Fe1 C3 H6 118.5 . . ? C4 C3 Fe1 70.4(3) . . ? C4 C3 H6 118.5 . . ? C4 C3 C2 121.2(5) . . ? C2 C3 Fe1 71.6(3) . . ? C2 C3 H6 118.5 . . ? Fe1 C2 H7 115.0 . . ? C3 C2 Fe1 67.9(3) . . ? C3 C2 H7 115.0 . . ? C3 C2 C1 123.6(5) . . ? C1 C2 Fe1 111.0(4) . . ? C1 C2 H7 115.0 . . ? O1 C1 C2 121.8(5) . . ? O1 C1 C7 120.5(5) . . ? C2 C1 C7 117.6(5) . . ? C1 C7 H9A 109.6 . . ? C1 C7 H9B 109.6 . . ? C1 C7 C6 110.1(4) . . ? H9A C7 H9B 108.2 . . ? C6 C7 H9A 109.6 . . ? C6 C7 H9B 109.6 . . ? P1 C6 H10 108.9 . . ? C5 C6 P1 107.6(4) . . ? C5 C6 C7 113.2(4) . . ? C5 C6 H10 108.9 . . ? C7 C6 P1 109.4(4) . . ? C7 C6 H10 108.9 . . ? C18 C17 P1 120.1(4) . . ? C22 C17 P1 119.7(4) . . ? C22 C17 C18 119.9(5) . . ? C17 C18 H12 119.6 . . ? C19 C18 C17 120.7(6) . . ? C19 C18 H12 119.6 . . ? C18 C19 C31 120.7(6) . . ? C18 C19 C20 117.6(6) . . ? C20 C19 C31 121.8(6) . . ? C19 C31 H14A 109.5 . . ? C19 C31 H14B 109.5 . . ? C19 C31 H14C 109.5 . . ? H14A C31 H14B 109.5 . . ? H14A C31 H14C 109.5 . . ? H14B C31 H14C 109.5 . . ? C19 C20 H15 118.9 . . ? C21 C20 C19 122.2(6) . . ? C21 C20 H15 118.9 . . ? C20 C21 H16 120.1 . . ? C20 C21 C22 119.7(6) . . ? C22 C21 H16 120.1 . . ? C17 C22 H17 120.0 . . ? C21 C22 C17 119.9(6) . . ? C21 C22 H17 120.0 . . ? C12 C11 P1 122.5(4) . . ? C16 C11 P1 117.6(4) . . ? C16 C11 C12 119.6(5) . . ? C11 C12 H19 119.6 . . ? C11 C12 C13 120.8(5) . . ? C13 C12 H19 119.6 . . ? C12 C13 C29 120.4(6) . . ? C14 C13 C12 117.6(5) . . ? C14 C13 C29 122.0(5) . . ? C13 C29 H21A 109.5 . . ? C13 C29 H21B 109.5 . . ? C13 C29 H21C 109.5 . . ? H21A C29 H21B 109.5 . . ? H21A C29 H21C 109.5 . . ? H21B C29 H21C 109.5 . . ? C13 C14 H22 118.9 . . ? C15 C14 C13 122.3(6) . . ? C15 C14 H22 118.9 . . ? C14 C15 H23 120.2 . . ? C16 C15 C14 119.6(6) . . ? C16 C15 H23 120.2 . . ? C11 C16 H24 120.0 . . ? C15 C16 C11 120.1(6) . . ? C15 C16 H24 120.0 . . ? C28 C23 P1 120.0(4) . . ? C24 C23 P1 119.4(4) . . ? C24 C23 C28 120.4(5) . . ? C23 C28 H26 119.9 . . ? C23 C28 C27 120.1(6) . . ? C27 C28 H26 119.9 . . ? C28 C27 C30 120.0(6) . . ? C26 C27 C28 118.3(5) . . ? C26 C27 C30 121.7(5) . . ? C27 C30 H28A 109.5 . . ? C27 C30 H28B 109.5 . . ? C27 C30 H28C 109.5 . . ? H28A C30 H28B 109.5 . . ? H28A C30 H28C 109.5 . . ? H28B C30 H28C 109.5 . . ? C27 C26 H29 119.3 . . ? C25 C26 C27 121.5(5) . . ? C25 C26 H29 119.3 . . ? C26 C25 H30 120.0 . . ? C26 C25 C24 120.0(6) . . ? C24 C25 H30 120.0 . . ? C23 C24 C25 119.6(6) . . ? C23 C24 H31 120.2 . . ? C25 C24 H31 120.2 . . ? F4 B1 F1 107.1(16) . . ? F2 B1 F4 111.3(15) . . ? F2 B1 F3 114.8(16) . . ? F2 B1 F1 105.5(17) . . ? F3 B1 F4 113.3(15) . . ? F3 B1 F1 103.9(15) . . ? F7 B2 F8 107.5(9) . . ? F5 B2 F7 108.5(9) . . ? F5 B2 F8 106.3(10) . . ? F6 B2 F7 111.2(9) . . ? F6 B2 F5 116.3(10) . . ? F6 B2 F8 106.6(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 C5 C4 C3 -52.8(5) . . . . ? Fe1 C5 C6 P1 178.0(3) . . . . ? Fe1 C5 C6 C7 57.1(6) . . . . ? Fe1 C4 C3 C2 -52.5(5) . . . . ? Fe1 C3 C2 C1 -101.2(5) . . . . ? Fe1 C2 C1 O1 106.8(5) . . . . ? Fe1 C2 C1 C7 -74.3(5) . . . . ? P1 C17 C18 C19 174.2(4) . . . . ? P1 C17 C22 C21 -173.3(4) . . . . ? P1 C11 C12 C13 -175.4(4) . . . . ? P1 C11 C16 C15 174.6(4) . . . . ? P1 C23 C28 C27 -174.2(4) . . . . ? P1 C23 C24 C25 175.2(4) . . . . ? O1 C1 C7 C6 -110.5(6) . . . . ? C5 C4 C3 Fe1 53.9(5) . . . . ? C5 C4 C3 C2 1.5(9) . . . . ? C4 C5 C6 P1 95.7(6) . . . . ? C4 C5 C6 C7 -25.3(8) . . . . ? C4 C3 C2 Fe1 51.9(5) . . . . ? C4 C3 C2 C1 -49.2(8) . . . . ? C3 C2 C1 O1 -176.5(5) . . . . ? C3 C2 C1 C7 2.4(8) . . . . ? C2 C1 C7 C6 70.6(6) . . . . ? C1 C7 C6 P1 -176.1(4) . . . . ? C1 C7 C6 C5 -56.2(6) . . . . ? C6 P1 C17 C18 -97.8(5) . . . . ? C6 P1 C17 C22 76.2(5) . . . . ? C6 P1 C11 C12 -14.5(5) . . . . ? C6 P1 C11 C16 171.4(4) . . . . ? C6 P1 C23 C28 -150.2(4) . . . . ? C6 P1 C23 C24 35.5(5) . . . . ? C6 C5 C4 Fe1 113.0(5) . . . . ? C6 C5 C4 C3 60.2(8) . . . . ? C17 P1 C6 C5 -62.5(4) . . . . ? C17 P1 C6 C7 60.9(4) . . . . ? C17 P1 C11 C12 -134.6(4) . . . . ? C17 P1 C11 C16 51.4(5) . . . . ? C17 P1 C23 C28 -31.2(5) . . . . ? C17 P1 C23 C24 154.6(4) . . . . ? C17 C18 C19 C31 179.5(6) . . . . ? C17 C18 C19 C20 -1.0(8) . . . . ? C18 C17 C22 C21 0.7(8) . . . . ? C18 C19 C20 C21 1.0(9) . . . . ? C19 C20 C21 C22 -0.1(10) . . . . ? C31 C19 C20 C21 -179.5(6) . . . . ? C20 C21 C22 C17 -0.7(9) . . . . ? C22 C17 C18 C19 0.2(8) . . . . ? C11 P1 C6 C5 176.9(4) . . . . ? C11 P1 C6 C7 -59.8(4) . . . . ? C11 P1 C17 C18 24.3(5) . . . . ? C11 P1 C17 C22 -161.7(4) . . . . ? C11 P1 C23 C28 87.9(5) . . . . ? C11 P1 C23 C24 -86.4(5) . . . . ? C11 C12 C13 C29 -178.8(5) . . . . ? C11 C12 C13 C14 1.9(7) . . . . ? C12 C11 C16 C15 0.4(8) . . . . ? C12 C13 C14 C15 -1.1(8) . . . . ? C13 C14 C15 C16 0.1(8) . . . . ? C29 C13 C14 C15 179.5(5) . . . . ? C14 C15 C16 C11 0.3(8) . . . . ? C16 C11 C12 C13 -1.5(8) . . . . ? C23 P1 C6 C5 57.5(4) . . . . ? C23 P1 C6 C7 -179.2(4) . . . . ? C23 P1 C17 C18 142.2(4) . . . . ? C23 P1 C17 C22 -43.9(5) . . . . ? C23 P1 C11 C12 106.2(5) . . . . ? C23 P1 C11 C16 -67.8(5) . . . . ? C23 C28 C27 C30 179.9(5) . . . . ? C23 C28 C27 C26 -1.5(8) . . . . ? C28 C23 C24 C25 1.0(8) . . . . ? C28 C27 C26 C25 2.1(8) . . . . ? C27 C26 C25 C24 -1.1(8) . . . . ? C30 C27 C26 C25 -179.3(5) . . . . ? C26 C25 C24 C23 -0.4(8) . . . . ? C24 C23 C28 C27 0.0(8) . . . . ? _smtbx_masks_special_details ; A solvent mask was calculated and 656 electrons were found in a volume of 2276\%A^3^ in 1 void per unit cell. This is consistent with the presence of 1[CH2Cl2] per formula unit which account for 672 electrons per unit cell. ; loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.250 0.000 -0.459 568.8 163.8 '4 DCM' 2 0.250 0.500 -0.786 568.8 163.8 '4 DCM' 3 0.750 0.000 -0.269 568.8 163.8 '4 DCM' 4 0.750 0.500 -0.980 568.8 163.8 '4 DCM' _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.045 _oxdiff_exptl_absorpt_empirical_full_min 0.954