#------------------------------------------------------------------------------ #$Date: 2020-02-04 05:13:16 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247531 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/39/4133977.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4133977 loop_ _publ_author_name 'Bear, Joseph C.' 'Cockcroft, Jeremy K.' 'Williams, Jeffrey H.' _publ_section_title ; Influence of Solvent in Crystal Engineering: A Significant Change to the Order-Disorder Transition in Ferrocene. ; _journal_issue 4 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 1731 _journal_page_last 1734 _journal_paper_doi 10.1021/jacs.9b11895 _journal_volume 142 _journal_year 2020 _chemical_formula_moiety '0.5(C20 H20 Fe2), C6 F6' _chemical_formula_sum 'C16 H10 F6 Fe' _chemical_formula_weight 372.09 _chemical_name_systematic Ferrocene:hexafluorobenzene _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-B 1' _space_group_name_H-M_alt 'B -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2019-08-29 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 76.621(6) _cell_angle_beta 77.687(6) _cell_angle_gamma 83.786(5) _cell_formula_units_Z 2 _cell_length_a 7.1670(4) _cell_length_b 9.2494(6) _cell_length_c 11.8880(10) _cell_measurement_reflns_used 3097 _cell_measurement_temperature 300 _cell_measurement_theta_max 26.4150 _cell_measurement_theta_min 4.6670 _cell_volume 747.60(9) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment C6F6 _diffrn_ambient_temperature 300 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2031 _diffrn_detector_type Atlas _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 18.00 88.00 1.00 2.00 -- 11.17-156.00 148.20 70 2 \w -10.00 19.00 1.00 2.00 -- 11.17 57.00-180.00 29 3 \w -13.00 85.00 1.00 2.00 -- 11.17 38.00 90.00 98 4 \w -17.00 84.00 1.00 2.00 -- 11.17 57.00 -60.00 101 5 \w -17.00 52.00 1.00 2.00 -- 11.17 -99.00 -90.00 69 6 \w -9.00 85.00 1.00 2.00 -- 11.17 38.00-150.00 94 7 \w -44.00 36.00 1.00 2.00 -- 11.17 -38.00 120.00 80 8 \w 10.00 69.00 1.00 2.00 -- 11.17-128.00 23.16 59 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0214813000 _diffrn_orient_matrix_UB_12 -0.0756339000 _diffrn_orient_matrix_UB_13 0.0254180000 _diffrn_orient_matrix_UB_21 -0.0297598000 _diffrn_orient_matrix_UB_22 0.0153672000 _diffrn_orient_matrix_UB_23 0.0571188000 _diffrn_orient_matrix_UB_31 -0.0946233000 _diffrn_orient_matrix_UB_32 -0.0167544000 _diffrn_orient_matrix_UB_33 0.0008568000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_unetI/netI 0.0264 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 5238 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 24.702 _diffrn_reflns_theta_max 24.702 _diffrn_reflns_theta_min 3.502 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.067 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.367 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 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_crystal_colour 'clear dark orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.653 _exptl_crystal_description block _exptl_crystal_F_000 372 _exptl_crystal_preparation 'Ferrocene dissolved in hot C6F6' _exptl_crystal_recrystallization_method 'Crystals grown using C6F6 as solvent in an NMR tube stood in hot water' _exptl_crystal_size_max 0.722 _exptl_crystal_size_mid 0.389 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.269 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.058 _refine_ls_extinction_coef 0.039(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 152 _refine_ls_number_reflns 1271 _refine_ls_number_restraints 190 _refine_ls_restrained_S_all 1.329 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0368 _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^)+(0.0582P)^2^+0.4392P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0994 _refine_ls_wR_factor_ref 0.1004 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1237 _reflns_number_total 1271 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja9b11895_si_002.cif _cod_data_source_block exp_1340 _cod_depositor_comments 'Adding full bibliography for 4133967--4133980.cif.' _cod_original_sg_number -1 _cod_original_sg_symbol_H-M '-B 1' _cod_database_code 4133977 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'Fe C16 H10 F6' _chemical_oxdiff_usercomment 'In capillary' _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. ; _shelx_estimated_absorpt_t_max 0.815 _shelx_estimated_absorpt_t_min 0.513 _reflns_odcompleteness_completeness 49.75 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Restrained distances C7-C9A \\sim C7-C10A \\sim C8-C10A \\sim C8-C11A \\sim C9-C11A \\sim C9-C7A \\sim C10-C7A \\sim C10-C8A ~ C11-C8A \\sim C11-C9A with sigma of 0.02 C7-C7A \\sim C8-C8A \\sim C9-C9A \\sim C10-C10A \\sim C11-C11A with sigma of 0.02 Fe1-C7 \\sim Fe1-C7A \\sim Fe1-C8 \\sim Fe1-C8A \\sim Fe1-C9 \\sim Fe1-C9A \\sim Fe1-C10 \\sim Fe1-C10A ~ Fe1-C11 \\sim Fe1-C11A with sigma of 0.02 3. Rigid bond restraints Fe1, C7, Fe1, C8, Fe1, C9, Fe1, C10, Fe1, C11, Fe1, C7A, Fe1, C8A, Fe1, C9A, Fe1, C10A, Fe1, C11A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Rigid body (RIGU) restrains C7, C9A, C7, C10A, C8, C10A, C8, C11A, C9, C11A, C9, C7A, C10, C7A, C10, C8A, C11, C8A, C11, C9A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Fixed Sof: C7(0.5) H7(0.5) C8(0.5) H8(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5) C11(0.5) H11(0.5) C7A(0.5) H7A(0.5) C8A(0.5) H8A(0.5) C9A(0.5) H9A(0.5) C10A(0.5) H10A(0.5) C11A(0.5) H11A(0.5) 6.a Aromatic/amide H refined with riding coordinates: C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A) ; _shelx_res_file ; exp_1340.res created by SHELXL-2014/7 TITL exp_1340 in -B 1 #-1 CELL 0.71073 7.167037 9.249421 11.888003 76.6212 77.6869 83.786 ZERR 2 0.000436 0.000578 0.000959 0.0061 0.006 0.0051 LATT 6 SFAC C H F Fe UNIT 32 20 12 2 SADI C7 C9A C7 C10A C8 C10A C8 C11A C9 C11A C9 C7A C10 C7A C10 C8A C11 C8A = C11 C9A SADI C7 C7A C8 C8A C9 C9A C10 C10A C11 C11A SADI Fe1 C7 Fe1 C7A Fe1 C8 Fe1 C8A Fe1 C9 Fe1 C9A Fe1 C10 Fe1 C10A Fe1 C11 = FE1 C11A DELU Fe1 C7 Fe1 C8 Fe1 C9 Fe1 C10 Fe1 C11 Fe1 C7A Fe1 C8A Fe1 C9A Fe1 C10A = FE1 C11A RIGU C7 C9A C7 C10A C8 C10A C8 C11A C9 C11A C9 C7A C10 C7A C10 C8A C11 C8A = C11 C9A L.S. 20 0 0 PLAN 1 SIZE 0.2 0.389 0.722 CONN 20 1.24 Fe1 BOND $H CONF list 4 fmap 2 53 acta SHEL 50 0.85 REM REM REM WGHT 0.058200 0.439200 EXTI 0.039317 FVAR 8.40757 FE1 4 0.250000 0.500000 0.250000 10.50000 0.07395 0.05267 = 0.05780 -0.00470 -0.02163 0.00369 PART 1 C7 1 0.315578 0.690456 0.128850 10.50000 0.10461 0.07117 = 0.08991 0.00804 -0.01562 -0.00977 AFIX 43 H7 2 0.433614 0.732446 0.107605 10.50000 -1.20000 AFIX 0 C8 1 0.256146 0.584778 0.076545 10.50000 0.09595 0.08516 = 0.05725 -0.00248 -0.01401 0.01105 AFIX 43 H8 2 0.328280 0.544632 0.014906 10.50000 -1.20000 AFIX 0 C9 1 0.069264 0.551732 0.134410 10.50000 0.08638 0.07810 = 0.05951 -0.01744 -0.02683 0.01376 AFIX 43 H9 2 -0.004646 0.485772 0.117542 10.50000 -1.20000 AFIX 0 C10 1 0.012279 0.634858 0.222107 10.50000 0.08604 0.06299 = 0.07467 -0.02015 -0.03466 0.01493 AFIX 43 H10 2 -0.105313 0.633772 0.273681 10.50000 -1.20000 AFIX 0 C11 1 0.165341 0.720011 0.217747 10.50000 0.09795 0.05319 = 0.08550 -0.00921 -0.03138 0.00858 AFIX 43 H11 2 0.166186 0.785493 0.266347 10.50000 -1.20000 AFIX 0 PART 0 F1 3 0.360730 0.981528 -0.120069 11.00000 0.09450 0.17257 = 0.13076 0.01622 0.01262 0.02241 F2 3 0.101504 0.812002 -0.148378 11.00000 0.22921 0.10240 = 0.10101 -0.04582 -0.04856 0.04510 F3 3 -0.259592 0.828915 -0.027231 11.00000 0.16351 0.12587 = 0.19534 -0.00953 -0.08700 -0.05285 C1 1 0.181045 0.990902 -0.061470 11.00000 0.07748 0.08466 = 0.07424 0.01024 -0.00712 0.01653 C2 1 0.048627 0.905438 -0.074792 11.00000 0.11862 0.06110 = 0.06925 -0.01243 -0.03043 0.01622 C3 1 -0.130589 0.914613 -0.014120 11.00000 0.09627 0.06856 = 0.09283 0.00354 -0.04011 -0.01055 PART 2 C7A 1 0.019041 0.584034 0.178357 10.50000 0.06949 0.09577 = 0.08561 -0.00591 -0.02422 0.00644 AFIX 43 H7A 2 -0.099588 0.543075 0.198160 10.50000 -1.20000 AFIX 0 C8A 1 0.079791 0.690597 0.232839 10.50000 0.07960 0.06748 = 0.07595 -0.00651 -0.01242 0.01760 AFIX 43 H8A 2 0.007690 0.731238 0.294223 10.50000 -1.20000 AFIX 0 C9A 1 0.268002 0.721035 0.175579 10.50000 0.08765 0.05424 = 0.05637 -0.01115 -0.00939 0.00614 AFIX 43 H9A 2 0.342520 0.785967 0.193173 10.50000 -1.20000 AFIX 0 C10A 1 0.325823 0.639405 0.088714 10.50000 0.08602 0.04820 = 0.05862 -0.01186 -0.01923 -0.00822 AFIX 43 H10A 2 0.444707 0.640745 0.038451 10.50000 -1.20000 AFIX 0 C11A 1 0.173756 0.553773 0.089346 10.50000 0.07574 0.06901 = 0.06032 -0.00359 -0.02563 -0.00854 AFIX 43 H11A 2 0.175213 0.488910 0.039894 10.50000 -1.20000 AFIX 0 HKLF 4 REM exp_1340 in -B 1 #-1 REM R1 = 0.0368 for 1237 Fo > 4sig(Fo) and 0.0377 for all 1271 data REM 152 parameters refined using 190 restraints END WGHT 0.0582 0.4392 REM Highest difference peak 0.269, deepest hole -0.211, 1-sigma level 0.058 Q1 1 -0.0549 0.8040 -0.0971 11.00000 0.05 0.27 ; _shelx_res_checksum 69721 _shelx_hkl_file ; 0 0 -2 7959.34 347.694 4 0 0 -2 8921.53 372.179 3 0 0 -4 7368.40 430.022 4 0 0 4 7873.59 444.037 4 0 0 4 7758.66 482.373 3 0 0 -4 8383.70 465.856 3 0 0 6 60925.8 2116.41 4 0 0 -6 65033.3 2107.66 3 0 0 -6 62891.1 2058.55 4 0 0 -8 25836.7 1214.29 3 0 0 8 26357.6 1383.82 3 0 0 -8 21663.3 1333.06 6 0 0 8 23613.8 1237.37 4 0 0 -10 11780.4 870.790 3 0 0 10 11263.3 918.221 4 0 0 12 5539.06 750.650 4 0 0 -12 6599.27 713.051 3 0 0 -14 305.371 245.281 3 0 0 14 92.8592 272.262 4 0 -1 14 793.029 362.840 4 0 1 -14 769.967 324.496 3 0 1 -12 3505.54 546.706 3 0 -1 12 3560.37 582.572 4 0 1 -10 5874.94 626.979 3 0 -1 10 4390.85 559.892 4 0 1 -8 842.922 238.533 3 0 1 -8 870.707 273.856 6 0 -1 8 1449.03 319.564 3 0 -1 8 795.332 214.262 4 0 -1 6 44132.0 1627.43 4 0 1 -6 49952.0 1762.87 3 0 -1 6 45643.1 1818.77 3 0 1 -4 30366.0 1144.04 3 0 -1 4 28209.8 1027.11 4 0 -1 4 30447.3 1194.95 3 0 -1 2 477854. 12671.1 7 0 1 -2 510013. 12713.8 3 0 -1 2 512167. 12760.2 6 0 -1 2 493901. 12739.6 3 0 -1 -2 498930. 12193.0 3 0 1 2 485318. 12331.2 4 0 1 4 223714. 5889.35 3 0 -1 -4 229560. 5837.83 3 0 1 4 220946. 5986.18 4 0 -1 -4 207404. 5889.54 4 0 -1 -6 98603.9 2881.05 3 0 -1 -6 91581.9 2934.97 4 0 1 6 92196.7 3030.81 4 0 -1 -8 65311.9 2263.04 3 0 -1 -8 62933.9 2294.99 4 0 1 8 67049.8 2511.46 3 0 1 8 61067.1 2433.91 4 0 -1 -10 4491.82 519.637 3 0 1 10 4239.12 617.840 4 0 -1 -10 4014.43 492.010 4 0 -1 -12 2780.87 487.051 3 0 1 12 3127.98 594.757 4 0 -1 -14 2144.09 467.324 3 0 1 14 2401.55 589.254 4 0 -2 12 1983.46 419.962 4 0 2 -12 1825.94 411.228 3 0 2 -10 6488.33 682.916 3 0 -2 10 5733.93 606.259 4 0 -2 8 8896.50 667.902 4 0 2 -8 9732.72 775.954 3 0 -2 8 11306.4 922.128 3 0 -2 8 9844.69 815.170 7 0 -2 6 65105.9 2132.40 4 0 2 -6 69970.3 2355.68 3 0 -2 6 64528.5 1763.91 8 0 -2 6 69291.6 2481.28 3 0 -2 4 54713.4 1910.11 7 0 2 -4 59284.3 1964.72 3 0 -2 4 56728.2 2012.84 3 0 -2 2 376078. 9584.74 3 0 2 -2 356819. 9555.26 6 0 -2 2 373378. 9500.65 7 0 2 -2 377606. 9562.04 3 0 2 -2 374151. 9463.24 7 0 -2 2 363582. 9561.73 6 0 2 0 248005. 6070.29 1 0 2 0 240172. 6236.26 6 0 -2 0 243457. 6236.93 6 0 2 0 253906. 6246.91 7 0 -2 0 242232. 6225.98 7 0 -2 0 255105. 6070.22 1 0 -2 0 228898. 6305.27 4 0 -2 -2 489816. 11450.8 5 0 -2 -2 475613. 11468.3 2 0 2 2 457996. 11757.7 4 0 2 2 465268. 11390.3 5 0 2 2 453124. 11450.0 2 0 -2 -4 792.143 137.431 5 0 -2 -4 794.079 222.945 4 0 2 4 865.994 266.116 4 0 -2 -6 155450. 4759.99 4 0 2 6 161977. 4922.82 4 0 -2 -6 168324. 4634.20 3 0 2 8 15510.2 1108.93 4 0 -2 -8 16664.3 1020.89 4 0 2 8 15640.2 1019.75 3 0 -2 -8 15299.1 914.379 3 0 -2 -10 4605.21 264.702 8 0 -2 -10 4642.18 552.837 3 0 -2 -10 4315.03 530.895 4 0 2 10 4070.56 640.911 4 0 2 12 5272.17 774.329 4 0 -2 -12 5709.35 668.508 3 0 2 14 1526.48 539.762 4 0 -2 -14 2065.65 445.697 3 0 -3 12 1890.58 401.152 4 0 3 -12 2149.13 444.776 3 0 -3 10 5890.55 603.212 4 0 3 -10 7147.48 755.851 3 0 -3 8 12079.0 766.044 4 0 -3 8 11738.1 923.110 7 0 3 -8 12062.2 901.127 3 0 -3 8 11268.0 394.020 8 0 -3 6 8793.53 750.557 3 0 -3 6 8429.82 432.040 8 0 3 -6 8149.15 677.105 3 0 3 -6 8606.91 752.854 6 0 -3 6 8864.10 586.228 4 0 -3 6 8802.66 694.548 7 0 3 -4 58867.5 2080.51 3 0 -3 4 59396.9 2128.68 3 0 -3 4 53151.7 2072.94 6 0 -3 4 55847.3 2004.59 7 0 -3 2 18384.8 846.358 7 0 3 -2 18655.4 910.750 3 0 -3 2 18114.8 891.810 6 0 -3 2 19027.5 742.824 1 0 3 -2 19791.9 858.589 7 0 -3 0 70855.0 1872.60 1 0 3 0 70316.7 2116.98 7 0 -3 0 70878.5 2094.54 7 0 3 0 68881.5 1873.50 1 0 -3 0 71453.4 2123.90 6 0 3 0 69168.2 2099.75 6 0 -3 0 69006.2 2216.74 4 0 3 2 29958.2 935.875 5 0 -3 -2 30484.0 974.142 5 0 3 2 28998.6 986.292 2 0 3 2 29041.3 1261.88 4 0 -3 -2 29669.9 1076.68 6 0 3 4 95517.8 3093.28 4 0 -3 -4 90010.6 2663.02 2 0 -3 -4 91429.4 2644.54 5 0 -3 -6 3210.34 447.504 4 0 -3 -6 3308.21 340.030 5 0 3 6 3278.32 545.266 4 0 3 8 27151.8 1578.85 4 0 -3 -8 25393.1 1420.18 4 0 3 8 28875.9 1419.79 3 0 -3 -8 28660.2 1225.57 5 0 3 10 13395.7 1156.69 4 0 -3 -10 12852.5 850.585 5 0 -3 -12 3210.70 477.274 5 0 3 12 3477.52 665.031 4 0 -3 -12 3612.54 263.582 8 0 3 14-157.180 319.262 4 0 -3 -14 848.720 292.554 5 0 3 16-40.8843 275.124 4 0 4 -12 788.397 322.983 3 0 -4 12 1272.28 448.272 1 0 4 -10 8765.13 865.967 3 0 -4 10 9471.17 769.429 4 0 -4 10 11132.5 1077.54 1 0 4 -8 6042.83 666.152 3 0 -4 8 6141.29 675.884 7 0 -4 8 7012.12 734.807 1 0 -4 8 5162.17 502.400 4 0 -4 8 5706.98 355.216 8 0 4 -6 17730.0 1109.06 3 0 -4 6 18812.2 831.946 8 0 4 -6 19695.4 1246.25 6 0 -4 6 20098.7 1165.75 7 0 -4 6 19479.2 1230.86 3 0 -4 6 19065.7 1108.69 1 0 4 -4 49054.5 1905.28 3 0 4 -4 45311.9 1723.79 7 0 -4 4 44856.3 1643.73 1 0 -4 4 41976.3 1874.14 6 0 4 -4 44854.1 1878.06 6 0 -4 2 102370. 3278.59 6 0 4 -2 105127. 3255.11 6 0 4 -2 107269. 3338.34 3 0 -4 2 106618. 2969.92 1 0 4 -2 107186. 3208.14 7 0 -4 2 108464. 3210.89 7 0 4 0 75731.3 2377.31 7 0 -4 0 76929.5 2385.58 6 0 4 0 74687.6 2347.31 6 0 -4 0 74260.5 2504.56 4 0 4 0 72792.8 2031.45 1 0 -4 0 78960.0 2341.02 7 0 4 2 103811. 3235.94 4 0 4 2 95426.6 2720.46 5 0 4 2 100041. 3000.02 7 0 -4 -2 102000. 2980.82 6 0 4 4 1521.06 366.236 4 0 4 4 1910.77 183.487 5 0 -4 -4 1748.25 236.787 5 0 -4 -6 23231.6 1381.71 4 0 -4 -6 26657.4 1126.67 5 0 4 6 25921.3 1475.67 4 0 -4 -6 26521.5 1133.88 2 0 4 8 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311.453 7 5 -6 -3 2868.09 633.343 6 -5 6 3 2663.00 411.618 3 -5 6 3 1793.57 471.921 7 -5 6 3 2072.68 341.208 1 -5 6 1 14113.5 889.659 3 -5 6 1 13845.3 1237.98 7 5 -6 -1 16850.2 1371.72 6 -5 6 -1 3837.72 653.341 7 -5 6 -1 3047.08 363.168 3 5 -6 1 3506.94 627.078 6 -5 6 -3 5748.05 466.577 5 -5 6 -3 6384.21 557.320 3 -5 6 -3 6470.59 833.481 7 5 -6 3 6714.02 870.974 6 -5 6 -5 6573.71 598.063 5 -5 6 -5 6722.77 573.908 3 -5 6 -5 7595.77 920.326 7 5 -6 5 5988.20 867.092 6 -5 6 -7 3120.94 477.585 5 -5 6 -7 2073.41 534.660 7 5 -6 7 3143.44 633.456 6 -5 6 -9 3598.72 584.459 5 -5 5 9 345.325 222.276 1 5 -5 -9 131.029 246.125 2 -5 5 9 482.083 312.617 7 5 -5 -7 132.693 257.290 6 5 -5 -7-124.458 276.060 2 -5 5 7 274.145 232.496 7 -5 5 7 23.9174 180.886 1 5 -5 -5 1891.50 507.548 6 5 -5 -5 1361.76 403.028 2 -5 5 5 1152.02 310.871 1 -5 5 5 642.281 315.363 7 -5 5 3 8949.34 746.338 3 -5 5 3 10257.0 1013.31 7 -5 5 3 8891.35 729.900 1 5 -5 -3 9195.77 1028.62 6 5 -5 -1 1724.58 441.721 6 -5 5 1 1668.30 276.059 1 -5 5 1 1244.03 376.301 7 5 -5 1 5473.77 433.854 1 -5 5 -1 5142.99 701.434 7 5 -5 1 6178.13 775.459 6 -5 5 -1 5789.40 459.793 3 5 -5 3 15079.4 789.769 1 -5 5 -3 16025.6 847.259 5 -5 5 -3 17788.8 867.576 3 -5 5 -3 16187.1 1285.13 7 -5 5 -5 2590.96 304.373 3 -5 5 -5 3138.50 416.436 5 -5 5 -5 3207.32 597.190 7 5 -5 5 2891.80 572.815 6 -5 5 -7 6687.35 719.838 5 -5 5 -7 7605.25 565.923 3 -5 5 -7 8415.85 949.274 7 5 -5 7 7363.83 911.281 6 -5 5 -9 4201.32 639.411 5 5 -5 9 5140.07 817.076 6 -5 5 -11 1230.17 417.449 5 -5 4 11 110.568 171.551 7 -5 4 9 31.2283 227.173 1 5 -4 -9 572.768 328.712 2 -5 4 9-65.8685 223.307 7 -5 4 7 1409.28 408.523 1 5 -4 -7 2629.83 610.219 6 5 -4 -7 2132.19 519.581 2 -5 4 7 1281.28 411.793 7 5 -4 -5 993.586 336.823 6 5 -4 -5 1429.20 433.645 2 -5 4 5 937.794 292.311 1 -5 4 5 1006.82 333.624 7 5 -4 -3 1963.71 487.650 6 5 -4 -3 1436.73 363.818 2 -5 4 3 1570.78 339.628 1 5 -4 -3 1560.23 176.713 5 -5 4 3 1680.81 320.625 3 -5 4 3 1808.39 428.758 7 -5 4 1 8812.02 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780.456 333.518 5 8 0 -6 50.9836 219.071 6 8 0 -4-255.192 276.029 6 8 0 -4 214.995 283.943 2 -8 0 4-118.836 266.730 1 8 0 -2 371.678 276.696 6 8 0 -2 773.523 377.559 2 -8 0 2 826.378 359.267 1 8 0 0 978.783 320.922 6 8 0 0 796.715 354.694 2 -8 0 0 665.239 291.682 1 -8 0 0 1233.61 306.054 7 8 0 0 882.915 257.959 4 -8 0 -2 2577.84 441.031 7 8 0 2 1718.53 374.392 4 8 0 2 2289.26 464.278 6 8 0 4 2610.75 474.365 4 8 0 4 2856.81 471.483 6 -8 0 -6 234.999 251.365 5 8 0 6 520.892 281.625 4 8 0 6 593.969 270.718 6 -8 0 -8 972.353 355.003 5 8 0 8 1218.20 418.642 4 8 0 8 750.401 292.061 6 -8 0 -10 872.954 396.692 5 8 1 -4 130.109 264.418 6 8 1 -4 120.294 316.749 2 -8 -1 4 504.537 323.997 1 8 1 -2 433.659 291.164 6 8 1 -2 675.319 362.155 2 -8 -1 2 228.261 231.076 1 8 1 0 1044.39 322.682 6 8 1 0 997.837 372.393 2 -8 -1 0 843.820 351.790 1 -8 -1 0 597.402 207.472 7 8 1 0 453.473 186.031 4 -8 -1 -2 1135.52 276.146 7 8 1 2 748.365 242.183 4 8 1 2 518.795 226.759 6 8 1 4 2229.39 433.752 4 8 1 4 2040.65 373.942 6 -8 -1 -6 1892.73 475.656 5 8 1 6 1492.77 396.460 4 8 1 6 1556.52 324.596 6 -8 -1 -8 651.366 333.015 5 8 1 8 1257.67 410.371 4 -8 -1 -10 363.898 304.529 5 8 2 -4 283.410 237.620 6 8 2 -4 64.0605 299.013 2 8 2 -2 750.620 282.583 6 8 2 -2 167.777 208.733 2 -8 -2 2 648.004 349.382 1 8 2 0 273.491 180.400 6 8 2 0 115.108 199.746 2 -8 -2 0 537.823 285.991 1 8 2 2 1585.70 369.040 2 8 2 2 904.085 278.961 4 8 2 2 1067.74 283.789 6 8 2 4 881.380 296.160 4 -8 -2 -6 1660.05 438.934 5 8 2 6 1718.32 421.003 4 -8 -2 -8 486.128 302.964 5 8 2 8 268.584 267.456 4 -8 -2 -10 563.495 326.117 5 8 2 10 1104.06 403.792 4 8 3 -4 404.332 330.286 2 8 3 -2 428.535 324.542 2 -8 -3 2-79.1213 247.056 1 8 3 0 1157.69 382.640 2 -8 -3 0 954.256 373.330 1 8 3 2 32.3436 150.856 2 8 3 2 280.260 208.696 4 8 3 4 1106.89 325.930 4 -8 -3 -6 801.963 333.624 5 8 3 6 185.216 200.216 4 -8 -3 -8 1123.98 422.739 5 8 3 8 826.743 354.966 4 8 3 10 305.174 318.607 4 8 4 -4 114.629 181.801 3 8 4 -2 388.940 270.929 2 8 4 -2 100.302 170.427 3 8 4 0 342.745 322.732 2 -8 -4 0-154.039 220.541 1 8 4 2 826.763 283.890 2 8 4 4 1041.44 340.375 4 8 4 6 305.887 300.578 4 -8 -4 -8 514.237 320.720 5 8 4 8 423.140 305.883 4 8 4 10 258.883 353.222 4 8 5 -2-57.7065 153.537 3 8 5 0 541.696 298.184 2 -8 -5 0-7.95717 167.463 1 8 5 2 90.5502 164.818 2 8 5 4 364.792 278.636 4 8 5 6 660.945 341.599 4 -8 -5 -8 710.118 384.243 5 8 5 8-199.511 293.353 4 8 5 10-2.24862 287.827 4 8 6 -2-337.818 222.798 3 -8 -6 -2 238.563 282.451 8 -8 -6 -4 846.513 352.929 8 -8 -6 -6 287.392 286.150 8 8 6 6 947.937 431.626 4 -8 -6 -8-79.7819 194.050 8 8 6 8-2.14785 318.279 4 8 6 10 225.602 404.625 4 8 7 8 187.192 355.611 4 -9 3 1 401.116 275.256 7 -9 3 -1 225.941 266.888 7 9 -3 1 418.794 272.968 6 -9 3 -3 346.505 264.617 7 9 -3 3 1.98427 174.174 6 9 -3 5 6.11065 184.649 6 9 -2 -1 302.655 217.098 6 -9 2 1-146.638 199.511 1 -9 2 -1 405.562 246.346 7 9 -2 1 417.862 286.604 6 -9 2 -3 282.470 191.053 7 9 -2 3-72.5721 241.994 6 -9 2 -5-171.374 183.264 7 9 -2 5-140.031 209.816 6 9 -2 5-74.0962 203.151 4 9 -1 -3 128.017 243.264 6 9 -1 -1 458.556 285.691 6 -9 1 1 220.784 246.516 1 9 -1 1 164.433 176.478 4 9 -1 1 260.525 230.155 6 -9 1 -3 784.865 286.027 7 9 -1 3 698.312 319.401 4 9 -1 3 409.885 256.562 6 9 -1 5 47.0963 221.281 4 -9 1 -7 437.068 288.345 5 9 0 -3 222.087 272.224 6 9 0 -1-675.800 357.833 2 -9 0 1 36.0477 198.014 1 9 0 1-3.04920 183.875 6 9 0 3 587.159 267.831 4 9 0 5 277.495 216.503 4 -9 0 -7-316.381 241.131 5 9 0 7 495.423 335.105 4 9 1 -1 1046.34 450.238 2 9 1 3 598.939 250.449 4 9 1 5 405.614 257.601 4 -9 -1 -7-106.248 211.097 5 9 1 7 392.900 261.984 4 9 2 -1 50.9146 264.977 2 9 2 1 411.399 241.454 2 9 2 5 944.700 357.950 4 -9 -2 -7 488.961 304.289 5 9 2 7-234.340 288.069 4 9 3 -1 185.126 210.270 2 9 3 1 295.137 256.857 2 9 3 5 547.413 303.163 4 9 3 7 276.816 230.733 4 9 4 -1 22.6966 212.309 2 9 4 7 194.438 253.534 4 0 0 0 0.00 0.00 0 TITL exp_1340 in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 7.167037 9.249421 11.888003 76.6212 77.6869 83.7860 ZERR 2.00 0.000436 0.000578 0.000959 0.0061 0.0060 0.0051 LATT 1 SFAC C H F Fe UNIT 32.00 20.00 12.00 2.00 TREF HKLF 4 END ; _shelx_hkl_checksum 4569 _olex2_date_sample_data_collection 2018-12-13 _olex2_exptl_crystal_mounting_method 'Inside 1.0 mm X-ray capillary' _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 2.016 _oxdiff_exptl_absorpt_empirical_full_min 0.792 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, y, z+1/2' '-x, -y, -z' '-x+1/2, -y, -z+1/2' 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 0.2500 0.5000 0.2500 0.0619(3) Uani 1 2 d DS TU P . . C7 C 0.3156(14) 0.6905(11) 0.1288(9) 0.093(3) Uani 0.5 1 d D U . A 1 H7 H 0.4336 0.7324 0.1076 0.112 Uiso 0.5 1 calc R . . A 1 C8 C 0.2561(15) 0.5848(12) 0.0765(7) 0.083(3) Uani 0.5 1 d D U . A 1 H8 H 0.3283 0.5446 0.0149 0.100 Uiso 0.5 1 calc R . . A 1 C9 C 0.0693(15) 0.5517(10) 0.1344(8) 0.074(2) Uani 0.5 1 d D U . A 1 H9 H -0.0046 0.4858 0.1175 0.088 Uiso 0.5 1 calc R . . A 1 C10 C 0.0123(12) 0.6349(10) 0.2221(8) 0.072(2) Uani 0.5 1 d D U . A 1 H10 H -0.1053 0.6338 0.2737 0.087 Uiso 0.5 1 calc R . . A 1 C11 C 0.1653(16) 0.7200(9) 0.2177(9) 0.079(2) Uani 0.5 1 d D U . A 1 H11 H 0.1662 0.7855 0.2663 0.095 Uiso 0.5 1 calc R . . A 1 F1 F 0.3607(3) 0.9815(4) -0.1201(3) 0.1483(11) Uani 1 1 d . . . . . F2 F 0.1015(5) 0.8120(3) -0.1484(2) 0.1419(10) Uani 1 1 d . . . . . F3 F -0.2596(5) 0.8289(3) -0.0272(3) 0.1544(11) Uani 1 1 d . . . . . C1 C 0.1810(5) 0.9909(4) -0.0615(3) 0.0861(10) Uani 1 1 d . . . . . C2 C 0.0486(6) 0.9054(3) -0.0748(3) 0.0831(9) Uani 1 1 d . . . . . C3 C -0.1306(5) 0.9146(4) -0.0141(3) 0.0856(9) Uani 1 1 d . . . . . C7A C 0.0190(11) 0.5840(13) 0.1784(10) 0.085(3) Uani 0.5 1 d D U . A 2 H7A H -0.0996 0.5431 0.1982 0.102 Uiso 0.5 1 calc R . . A 2 C8A C 0.0798(14) 0.6906(11) 0.2328(9) 0.078(2) Uani 0.5 1 d D U . A 2 H8A H 0.0077 0.7312 0.2942 0.094 Uiso 0.5 1 calc R . . A 2 C9A C 0.2680(14) 0.7210(8) 0.1756(7) 0.0677(19) Uani 0.5 1 d D U . A 2 H9A H 0.3425 0.7860 0.1932 0.081 Uiso 0.5 1 calc R . . A 2 C10A C 0.3258(11) 0.6394(8) 0.0887(6) 0.0631(17) Uani 0.5 1 d D U . A 2 H10A H 0.4447 0.6407 0.0385 0.076 Uiso 0.5 1 calc R . . A 2 C11A C 0.1738(15) 0.5538(10) 0.0893(8) 0.068(2) Uani 0.5 1 d D U . A 2 H11A H 0.1752 0.4889 0.0399 0.081 Uiso 0.5 1 calc R . . 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 Fe1 0.0740(4) 0.0527(4) 0.0578(4) -0.0047(2) -0.0216(3) 0.0037(2) C7 0.105(5) 0.071(9) 0.090(10) 0.008(4) -0.016(4) -0.010(5) C8 0.096(7) 0.085(9) 0.057(4) -0.002(4) -0.014(5) 0.011(5) C9 0.086(6) 0.078(4) 0.060(7) -0.017(4) -0.027(4) 0.014(5) C10 0.086(4) 0.063(6) 0.075(5) -0.020(3) -0.035(3) 0.015(3) C11 0.098(8) 0.053(4) 0.085(7) -0.009(5) -0.031(5) 0.009(6) F1 0.0945(15) 0.173(3) 0.131(2) 0.0162(18) 0.0126(14) 0.0224(15) F2 0.229(3) 0.1024(17) 0.1010(17) -0.0458(14) -0.0486(18) 0.0451(18) F3 0.164(2) 0.126(2) 0.195(3) -0.0095(19) -0.087(2) -0.0528(19) C1 0.077(2) 0.085(2) 0.074(2) 0.0102(17) -0.0071(16) 0.0165(17) C2 0.119(3) 0.0611(17) 0.0693(19) -0.0124(14) -0.0304(18) 0.0162(18) C3 0.096(2) 0.0686(19) 0.093(2) 0.0035(17) -0.040(2) -0.0105(17) C7A 0.069(4) 0.096(9) 0.086(9) -0.006(4) -0.024(4) 0.006(4) C8A 0.080(6) 0.067(8) 0.076(4) -0.007(4) -0.012(5) 0.018(4) C9A 0.088(5) 0.054(3) 0.056(6) -0.011(3) -0.009(4) 0.006(4) C10A 0.086(4) 0.048(5) 0.059(4) -0.012(3) -0.019(3) -0.008(3) C11A 0.076(6) 0.069(4) 0.060(5) -0.004(4) -0.026(4) -0.009(5) 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 2 16 0.1688 -2 -11 3 0.3527 -2 10 12 0.1016 1 -7 -15 0.1000 0 11 -6 0.1527 -1 7 15 0.1000 -7 7 -8 0.1653 8 -2 10 0.2091 2 -8 10 0.2361 -5 2 -14 0.1401 1 6 -12 0.1415 0 -5 13 0.2332 -5 10 1 0.1680 8 0 12 0.2066 1 -9 -13 0.1120 3 -12 -3 0.2141 3 -11 5 0.2285 6 -9 6 0.2201 -8 5 -7 0.1646 7 6 -6 0.2193 2 13 4 0.1666 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 C7 Fe1 C7 180.0 4_565 . C7 Fe1 C9 68.2(4) . . C7 Fe1 C9 111.8(4) . 4_565 C7 Fe1 C9 111.8(4) 4_565 . C7 Fe1 C9 68.2(4) 4_565 4_565 C7 Fe1 C10 112.0(4) 4_565 . C7 Fe1 C10 68.0(4) . . C7 Fe1 C10 112.0(4) . 4_565 C7 Fe1 C10 68.0(4) 4_565 4_565 C7 Fe1 C11 139.9(3) 4_565 . C7 Fe1 C11 40.1(3) 4_565 4_565 C7 Fe1 C11 139.9(3) . 4_565 C7 Fe1 C11 40.1(3) . . C8 Fe1 C7 41.0(4) 4_565 4_565 C8 Fe1 C7 139.0(4) . 4_565 C8 Fe1 C7 41.0(4) . . C8 Fe1 C7 139.0(4) 4_565 . C8 Fe1 C8 180.0 4_565 . C8 Fe1 C9 40.4(3) . . C8 Fe1 C9 139.6(3) 4_565 . C8 Fe1 C9 139.6(3) . 4_565 C8 Fe1 C9 40.4(3) 4_565 4_565 C8 Fe1 C10 111.9(4) 4_565 . C8 Fe1 C10 68.1(4) . . C8 Fe1 C10 68.1(4) 4_565 4_565 C8 Fe1 C10 111.9(4) . 4_565 C8 Fe1 C11 68.0(4) . . C8 Fe1 C11 68.0(4) 4_565 4_565 C8 Fe1 C11 112.0(4) . 4_565 C8 Fe1 C11 112.0(4) 4_565 . C9 Fe1 C9 180.0(4) 4_565 . C9 Fe1 C10 139.7(3) . 4_565 C9 Fe1 C10 139.7(3) 4_565 . C9 Fe1 C10 40.3(3) 4_565 4_565 C9 Fe1 C10 40.3(3) . . C9 Fe1 C11 67.7(4) 4_565 4_565 C9 Fe1 C11 67.7(4) . . C9 Fe1 C11 112.3(4) . 4_565 C9 Fe1 C11 112.3(4) 4_565 . C10 Fe1 C10 180.0 . 4_565 C11 Fe1 C10 139.7(3) 4_565 . C11 Fe1 C10 40.3(3) . . C11 Fe1 C10 40.3(3) 4_565 4_565 C11 Fe1 C10 139.7(3) . 4_565 C11 Fe1 C11 180.0(6) 4_565 . C7A Fe1 C7A 180.0 4_565 . C7A Fe1 C8A 41.8(4) . . C7A Fe1 C8A 138.2(4) 4_565 . C7A Fe1 C8A 41.8(4) 4_565 4_565 C7A Fe1 C8A 138.2(4) . 4_565 C7A Fe1 C9A 111.4(4) . 4_565 C7A Fe1 C9A 68.6(4) . . C7A Fe1 C9A 68.6(4) 4_565 4_565 C7A Fe1 C9A 111.4(4) 4_565 . C7A Fe1 C10A 68.3(4) . . C7A Fe1 C10A 111.7(4) . 4_565 C7A Fe1 C10A 111.7(4) 4_565 . C7A Fe1 C10A 68.3(4) 4_565 4_565 C7A Fe1 C11A 40.8(3) . . C7A Fe1 C11A 139.2(3) . 4_565 C7A Fe1 C11A 40.8(3) 4_565 4_565 C7A Fe1 C11A 139.2(3) 4_565 . C8A Fe1 C8A 180.0(7) 4_565 . C8A Fe1 C9A 139.7(3) 4_565 . C8A Fe1 C9A 40.3(3) 4_565 4_565 C8A Fe1 C9A 139.7(3) . 4_565 C8A Fe1 C9A 40.3(3) . . C8A Fe1 C10A 112.2(3) 4_565 . C8A Fe1 C10A 112.2(3) . 4_565 C8A Fe1 C10A 67.8(3) . . C8A Fe1 C10A 67.8(3) 4_565 4_565 C8A Fe1 C11A 69.0(4) . . C8A Fe1 C11A 69.0(4) 4_565 4_565 C8A Fe1 C11A 111.0(4) 4_565 . C8A Fe1 C11A 111.0(4) . 4_565 C9A Fe1 C9A 180.0(5) 4_565 . C9A Fe1 C10A 140.4(3) . 4_565 C9A Fe1 C10A 39.6(3) . . C9A Fe1 C10A 140.4(3) 4_565 . C9A Fe1 C10A 39.6(3) 4_565 4_565 C10A Fe1 C10A 180.0 4_565 . C11A Fe1 C9A 112.2(3) . 4_565 C11A Fe1 C9A 112.2(3) 4_565 . C11A Fe1 C9A 67.8(3) . . C11A Fe1 C9A 67.8(3) 4_565 4_565 C11A Fe1 C10A 40.5(3) . . C11A Fe1 C10A 139.5(3) . 4_565 C11A Fe1 C10A 139.5(3) 4_565 . C11A Fe1 C10A 40.5(3) 4_565 4_565 C11A Fe1 C11A 180.0 . 4_565 Fe1 C7 H7 126.0 . . C8 C7 Fe1 69.3(5) . . C8 C7 H7 126.2 . . C11 C7 Fe1 70.1(5) . . C11 C7 H7 126.2 . . C11 C7 C8 107.6(8) . . Fe1 C8 H8 125.6 . . C7 C8 Fe1 69.8(5) . . C7 C8 H8 126.2 . . C9 C8 Fe1 70.0(4) . . C9 C8 C7 107.6(7) . . C9 C8 H8 126.2 . . Fe1 C9 H9 126.0 . . C8 C9 Fe1 69.5(5) . . C8 C9 H9 125.8 . . C8 C9 C10 108.5(8) . . C10 C9 Fe1 70.2(4) . . C10 C9 H9 125.8 . . Fe1 C10 H10 126.3 . . C9 C10 Fe1 69.4(4) . . C9 C10 H10 126.3 . . C9 C10 C11 107.4(8) . . C11 C10 Fe1 69.5(4) . . C11 C10 H10 126.3 . . Fe1 C11 H11 126.1 . . C7 C11 Fe1 69.8(5) . . C7 C11 C10 108.9(8) . . C7 C11 H11 125.6 . . C10 C11 Fe1 70.1(4) . . C10 C11 H11 125.6 . . F1 C1 C2 120.5(4) . . F1 C1 C3 119.8(4) . 3_575 C2 C1 C3 119.7(3) . 3_575 F2 C2 C1 118.8(4) . . C3 C2 F2 121.3(4) . . C3 C2 C1 119.8(3) . . F3 C3 C1 120.2(4) . 3_575 F3 C3 C2 119.3(4) . . C2 C3 C1 120.5(3) . 3_575 Fe1 C7A H7A 125.7 . . C8A C7A Fe1 69.3(5) . . C8A C7A H7A 126.4 . . C11A C7A Fe1 70.1(4) . . C11A C7A H7A 126.4 . . C11A C7A C8A 107.1(7) . . Fe1 C8A H8A 126.0 . . C7A C8A Fe1 68.8(5) . . C7A C8A H8A 126.5 . . C9A C8A Fe1 70.2(4) . . C9A C8A C7A 107.0(7) . . C9A C8A H8A 126.5 . . Fe1 C9A H9A 126.2 . . C8A C9A Fe1 69.5(5) . . C8A C9A H9A 125.3 . . C10A C9A Fe1 70.6(4) . . C10A C9A C8A 109.4(7) . . C10A C9A H9A 125.3 . . Fe1 C10A H10A 126.9 . . C9A C10A Fe1 69.7(4) . . C9A C10A H10A 125.8 . . C9A C10A C11A 108.5(7) . . C11A C10A Fe1 69.2(4) . . C11A C10A H10A 125.8 . . Fe1 C11A H11A 126.2 . . C7A C11A Fe1 69.1(5) . . C7A C11A H11A 126.0 . . C10A C11A Fe1 70.3(4) . . C10A C11A C7A 108.0(7) . . C10A C11A H11A 126.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Fe1 C7 2.029(8) . Fe1 C7 2.029(8) 4_565 Fe1 C8 2.022(8) 4_565 Fe1 C8 2.022(8) . Fe1 C9 2.029(8) . Fe1 C9 2.029(8) 4_565 Fe1 C10 2.039(7) 4_565 Fe1 C10 2.039(7) . Fe1 C11 2.032(8) . Fe1 C11 2.032(8) 4_565 Fe1 C7A 2.021(8) 4_565 Fe1 C7A 2.021(8) . Fe1 C8A 2.028(8) . Fe1 C8A 2.028(8) 4_565 Fe1 C9A 2.037(7) . Fe1 C9A 2.037(7) 4_565 Fe1 C10A 2.049(7) . Fe1 C10A 2.049(7) 4_565 Fe1 C11A 2.035(8) 4_565 Fe1 C11A 2.035(8) . C7 H7 0.9300 . C7 C8 1.417(12) . C7 C11 1.391(12) . C8 H8 0.9300 . C8 C9 1.400(11) . C9 H9 0.9300 . C9 C10 1.402(10) . C10 H10 0.9300 . C10 C11 1.404(11) . C11 H11 0.9300 . F1 C1 1.331(4) . F2 C2 1.339(4) . F3 C3 1.336(4) . C1 C2 1.355(5) . C1 C3 1.363(5) 3_575 C2 C3 1.337(5) . C3 C1 1.363(5) 3_575 C7A H7A 0.9300 . C7A C8A 1.445(12) . C7A C11A 1.413(11) . C8A H8A 0.9300 . C8A C9A 1.401(11) . C9A H9A 0.9300 . C9A C10A 1.385(9) . C10A H10A 0.9300 . C10A C11A 1.413(10) . C11A H11A 0.9300 . 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_4 Fe1 C7 C8 C9 60.1(6) . . Fe1 C7 C11 C10 -59.5(6) . . Fe1 C8 C9 C10 59.6(6) . . Fe1 C9 C10 C11 59.4(6) . . Fe1 C10 C11 C7 59.3(6) . . Fe1 C7A C8A C9A 60.1(6) . . Fe1 C7A C11A C10A -59.8(6) . . Fe1 C8A C9A C10A 59.5(6) . . Fe1 C9A C10A C11A 58.5(6) . . Fe1 C10A C11A C7A 59.0(6) . . C7 C8 C9 Fe1 -59.9(6) . . C7 C8 C9 C10 -0.2(10) . . C8 C7 C11 Fe1 59.4(6) . . C8 C7 C11 C10 -0.1(10) . . C8 C9 C10 Fe1 -59.2(6) . . C8 C9 C10 C11 0.2(10) . . C9 C10 C11 Fe1 -59.3(6) . . C9 C10 C11 C7 -0.1(10) . . C11 C7 C8 Fe1 -59.9(6) . . C11 C7 C8 C9 0.2(10) . . F1 C1 C2 F2 -0.3(5) . . F1 C1 C2 C3 179.1(3) . . F2 C2 C3 F3 -0.1(5) . . F2 C2 C3 C1 179.2(3) . 3_575 C1 C2 C3 F3 -179.5(3) . . C1 C2 C3 C1 -0.2(5) . 3_575 C3 C1 C2 F2 -179.2(3) 3_575 . C3 C1 C2 C3 0.2(5) 3_575 . C7A C8A C9A Fe1 -59.3(6) . . C7A C8A C9A C10A 0.2(10) . . C8A C7A C11A Fe1 59.7(6) . . C8A C7A C11A C10A -0.1(10) . . C8A C9A C10A Fe1 -58.8(6) . . C8A C9A C10A C11A -0.3(10) . . C9A C10A C11A Fe1 -58.8(6) . . C9A C10A C11A C7A 0.2(9) . . C11A C7A C8A Fe1 -60.2(6) . . C11A C7A C8A C9A -0.1(10) . . 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 -0.2686 2.3142 16.2646 0.2326 0.9726 0.0006 -2.3171 -11.4787 3.4347 0.9057 0.0887 0.4145 -1.5710 10.0117 11.7178 -0.4931 0.8699 -0.0090 1.0583 -7.2680 -14.6455 0.2002 -0.9797 0.0091 0.3919 10.8243 -5.8249 -0.9583 -0.1780 -0.2234 -1.0583 7.2680 14.6455 -0.2002 0.9797 -0.0091 -6.5258 6.7262 -8.0051 -0.8524 -0.1597 0.4979 8.3870 -2.3006 9.8500 0.6045 0.2777 -0.7466 1.7194 -8.0616 10.3378 0.9094 0.4154 -0.0188 -5.4931 2.1471 -14.0868 -0.6385 -0.6081 0.4717 1.4474 5.5371 -12.4381 -0.7039 -0.6684 -0.2404 0.2367 -4.9595 13.4864 0.7230 0.6871 0.0723 -5.4180 10.1821 0.7090 -0.8685 0.3582 0.3427 7.9371 -0.0535 12.2859 0.4868 0.4647 -0.7396 0.5511 -9.3606 -13.2918 0.3820 -0.9195 0.0933 3.2162 -11.8266 -2.8979 0.8899 -0.4430 -0.1087 2.8729 -10.7198 4.8494 0.9958 0.0268 -0.0881 5.5526 -8.7743 5.6806 0.9273 0.0244 -0.3735 -8.2507 4.8523 -6.8016 -0.7171 -0.0684 0.6936 6.7252 6.2261 -6.1860 -0.4837 -0.4578 -0.7460 2.0871 12.9699 3.7033 -0.8420 0.3487 -0.4116