##################################################################### data_PCN-168-100K _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H32.67 Fe2 O10.67' _chemical_formula_weight 951.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 192 _space_group_name_H-M_alt 'P 6/m c c' _space_group_name_Hall '-P 6 2c' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 28.8591(9) _cell_length_b 28.859 _cell_length_c 35.5304(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 25626.9(19) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9985 _cell_measurement_theta_min 2.4871 _cell_measurement_theta_max 45.8403 _exptl_crystal_description Rod-like _exptl_crystal_colour Dark-red _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 0.370 _exptl_crystal_F_000 2928 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 1.499 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.2950 _exptl_absorpt_correction_T_max 0.7490 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3722 _diffrn_reflns_av_unetI/netI 0.0438 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.487 _diffrn_reflns_theta_max 45.990 _diffrn_reflns_theta_full 45.990 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 3722 _reflns_number_gt 2712 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _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. ; _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2014)' _computing_publication_material 'SHELXTL (Sheldrick, 2014)' _refine_special_details ; ? ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.004 -0.006 -0.004 21204 6816 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1056P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3722 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1470 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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_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 0.40673(2) 0.72143(2) 0.0000 0.0449(3) Uani 1 2 d S T P . . O1 O 0.36713(11) 0.60272(10) 0.04062(7) 0.0759(8) Uani 1 1 d . . . . . O2 O 0.42764(9) 0.68730(11) 0.04012(7) 0.0772(8) Uani 1 1 d . . . . . O3 O 0.3333 0.6667 0.0000 0.0364(11) Uani 1 6 d S T P . . O4 O 0.48547(10) 0.78072(10) 0.0000 0.0612(9) Uani 1 2 d S T P . . C1 C 0.40734(15) 0.64153(16) 0.05382(11) 0.0514(9) Uani 1 1 d . . . . . C2 C 0.43322(15) 0.63288(16) 0.08540(11) 0.0496(9) Uani 1 1 d . . . . . C3 C 0.4756(2) 0.67259(19) 0.10239(15) 0.1125(15) Uani 1 1 d . . . . . H3 H 0.4889 0.7081 0.0936 0.135 Uiso 1 1 calc R U . . . C4 C 0.50164(17) 0.6638(2) 0.13296(14) 0.1109(15) Uani 1 1 d . . . . . H4 H 0.5317 0.6937 0.1440 0.133 Uiso 1 1 calc R U . . . C5 C 0.48559(16) 0.61567(18) 0.14663(10) 0.0584(10) Uani 1 1 d . . . . . C6 C 0.4437(2) 0.5754(2) 0.12877(17) 0.1252(17) Uani 1 1 d . . . . . H6 H 0.4325 0.5394 0.1355 0.150 Uiso 1 1 calc R U . . . C7 C 0.41735(19) 0.5853(2) 0.10128(17) 0.1272(17) Uani 1 1 d . . . . . H7 H 0.3848 0.5559 0.0925 0.153 Uiso 1 1 calc R U . . . C8 C 0.51273(14) 0.60622(15) 0.17768(11) 0.0599(10) Uani 1 1 d . . . . . C9 C 0.56411(17) 0.64544(15) 0.18746(11) 0.0799(11) Uani 1 1 d . . . . . H9 H 0.5804 0.6788 0.1747 0.096 Uiso 1 1 calc R U . . . C10 C 0.59210(15) 0.63670(17) 0.21561(12) 0.0874(12) Uani 1 1 d . . . . . H10 H 0.6278 0.6636 0.2211 0.105 Uiso 1 1 calc R U . . . C11 C 0.56868(14) 0.58875(14) 0.23625(9) 0.0581(10) Uani 1 1 d . . . . . C12 C 0.51730(13) 0.54957(12) 0.22649(9) 0.0516(9) Uani 1 1 d . . . . . C13 C 0.49003(12) 0.55786(13) 0.19839(10) 0.0545(9) Uani 1 1 d . . . . . H13 H 0.4547 0.5303 0.1926 0.065 Uiso 1 1 calc R U . . . C14 C 0.5000 0.5000 0.2500 0.0451(16) Uani 1 4 d S T P . . 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 0.0541(5) 0.0531(5) 0.0283(6) 0.000 0.000 0.0275(4) O1 0.0948(18) 0.0727(17) 0.056(2) 0.0021(14) -0.0097(15) 0.0386(16) O2 0.0715(16) 0.0839(18) 0.062(2) 0.0073(15) -0.0109(14) 0.0282(14) O3 0.0496(16) 0.0496(16) 0.010(3) 0.000 0.000 0.0248(8) O4 0.0619(19) 0.0674(19) 0.049(2) 0.000 0.000 0.0283(16) C1 0.059(2) 0.060(3) 0.031(3) -0.004(2) -0.002(2) 0.026(2) C2 0.057(2) 0.055(2) 0.030(3) 0.005(2) -0.002(2) 0.023(2) C3 0.124(4) 0.103(4) 0.099(4) 0.026(3) -0.021(3) 0.049(4) C4 0.109(3) 0.099(4) 0.098(4) -0.001(3) -0.032(3) 0.032(3) C5 0.066(3) 0.068(3) 0.036(3) 0.004(3) -0.008(2) 0.030(2) C6 0.133(4) 0.107(4) 0.116(5) 0.020(4) -0.032(4) 0.046(4) C7 0.114(4) 0.111(5) 0.120(5) 0.008(4) -0.036(4) 0.028(3) C8 0.064(3) 0.069(3) 0.044(3) -0.004(2) -0.005(2) 0.031(2) C9 0.095(3) 0.076(3) 0.064(3) 0.012(2) -0.004(3) 0.039(3) C10 0.076(3) 0.103(3) 0.073(3) 0.005(3) -0.013(3) 0.037(3) C11 0.069(2) 0.061(2) 0.041(3) 0.009(2) -0.0047(19) 0.0301(18) C12 0.058(2) 0.069(2) 0.030(3) -0.0004(19) -0.0029(19) 0.034(2) C13 0.052(2) 0.056(2) 0.046(3) -0.003(2) -0.001(2) 0.0198(18) C14 0.062(3) 0.062(3) 0.025(4) 0.000 0.000 0.041(4) _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 O3 1.9070(6) . ? Fe1 O2 1.990(3) . ? Fe1 O2 1.990(3) 16 ? Fe1 O1 2.009(3) 3_665 ? Fe1 O1 2.009(3) 18_665 ? Fe1 O4 2.050(3) . ? O1 C1 1.233(3) . ? O1 Fe1 2.009(3) 14_565 ? O2 C1 1.245(4) . ? O3 Fe1 1.9070(6) 3_665 ? O3 Fe1 1.9070(6) 14_565 ? C1 C2 1.437(4) . ? C2 C3 1.332(5) . ? C2 C7 1.336(5) . ? C3 C4 1.413(5) . ? C4 C5 1.318(5) . ? C5 C6 1.345(5) . ? C5 C8 1.455(4) . ? C6 C7 1.354(6) . ? C8 C9 1.386(4) . ? C8 C13 1.416(4) . ? C9 C10 1.386(5) . ? C10 C11 1.405(4) . ? C11 C12 1.386(4) . ? C11 C11 1.400(6) 9 ? C12 C13 1.364(4) . ? C12 C14 1.510(3) . ? C14 C12 1.510(3) 9 ? C14 C12 1.510(3) 4_665 ? C14 C12 1.510(3) 10_665 ? 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 O3 Fe1 O2 94.35(7) . . ? O3 Fe1 O2 94.35(7) . 16 ? O2 Fe1 O2 91.51(15) . 16 ? O3 Fe1 O1 94.26(7) . 3_665 ? O2 Fe1 O1 87.67(10) . 3_665 ? O2 Fe1 O1 171.39(9) 16 3_665 ? O3 Fe1 O1 94.26(7) . 18_665 ? O2 Fe1 O1 171.39(9) . 18_665 ? O2 Fe1 O1 87.66(10) 16 18_665 ? O1 Fe1 O1 91.87(14) 3_665 18_665 ? O3 Fe1 O4 179.58(8) . . ? O2 Fe1 O4 85.95(9) . . ? O2 Fe1 O4 85.95(9) 16 . ? O1 Fe1 O4 85.44(9) 3_665 . ? O1 Fe1 O4 85.44(9) 18_665 . ? C1 O1 Fe1 134.4(2) . 14_565 ? C1 O2 Fe1 135.0(2) . . ? Fe1 O3 Fe1 119.998(2) 3_665 . ? Fe1 O3 Fe1 120.000(1) 3_665 14_565 ? Fe1 O3 Fe1 120.0 . 14_565 ? O1 C1 O2 123.0(4) . . ? O1 C1 C2 118.3(4) . . ? O2 C1 C2 118.7(3) . . ? C3 C2 C7 112.9(4) . . ? C3 C2 C1 122.6(4) . . ? C7 C2 C1 124.6(4) . . ? C2 C3 C4 122.4(4) . . ? C5 C4 C3 122.3(4) . . ? C4 C5 C6 115.3(4) . . ? C4 C5 C8 122.6(4) . . ? C6 C5 C8 122.0(4) . . ? C5 C6 C7 120.9(4) . . ? C2 C7 C6 125.6(4) . . ? C9 C8 C13 117.0(3) . . ? C9 C8 C5 119.5(4) . . ? C13 C8 C5 123.5(4) . . ? C10 C9 C8 121.0(3) . . ? C9 C10 C11 121.2(3) . . ? C12 C11 C11 109.40(19) . 9 ? C12 C11 C10 117.7(3) . . ? C11 C11 C10 132.6(2) 9 . ? C13 C12 C11 121.0(3) . . ? C13 C12 C14 128.6(3) . . ? C11 C12 C14 110.3(3) . . ? C12 C13 C8 122.0(3) . . ? C12 C14 C12 115.4(2) 9 4_665 ? C12 C14 C12 112.8(2) 9 10_665 ? C12 C14 C12 100.5(3) 4_665 10_665 ? C12 C14 C12 100.5(3) 9 . ? C12 C14 C12 112.8(2) 4_665 . ? C12 C14 C12 115.4(2) 10_665 . ? _refine_diff_density_max 0.249 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.031 _shelx_res_file ; C:\PCN-168\100K\PCN-168-100K.res created by SHELXL-2014/7 REM reset to P6/mcc #192 REM REM REM REM p in P6/mcc #192 REM R1 = 0.2947 for 2920 Fo > 4sig(Fo) and 0.3220 for all 3722 data REM 69 parameters refined using 0 restraints REM Highest difference peak 2.685, deepest hole -2.137, 1-sigma level 0.209 REM p in P6/mcc #192 REM R1 = 0.2947 for 2920 Fo > 4sig(Fo) and 0.3220 for all 3722 data REM 69 parameters refined using 0 restraints REM Highest difference peak 2.685, deepest hole -2.137, 1-sigma level 0.209 REM p in P6/mcc #192 REM R1 = 0.0837 for 2712 Fo > 4sig(Fo) and 0.0912 for all 3722 data REM 69 parameters refined using 0 restraints REM Highest difference peak 0.787, deepest hole -0.911, 1-sigma level 0.044 TITL p in P6/mcc #192 CELL 1.54184 28.8591 28.8591 35.5304 90.000 90.000 120.000 ZERR 6.0000 0.0009 0.0000 0.0013 0.000 0.000 0.000 LATT 1 SYMM X-Y, X, Z SYMM -Y, X-Y, Z SYMM -X, -Y, Z SYMM -X+Y, -X, Z SYMM Y, -X+Y, Z SYMM X-Y, -Y, 0.5-Z SYMM -X, -X+Y, 0.5-Z SYMM Y, X, 0.5-Z SYMM -Y, -X, 0.5-Z SYMM -X+Y, Y, 0.5-Z SYMM X, X-Y, 0.5-Z SFAC C H O FE UNIT 318 196.0002 64.0002 12 MERG 2 FMAP 2 GRID PLAN 20 TEMP -173 BOND L.S. 20 ACTA WGHT 0.105600 FVAR 1.88130 FE1 4 0.406729 0.721432 0.000000 10.50000 0.05408 0.05315 = 0.02827 0.00000 0.00000 0.02748 O1 3 0.367131 0.602718 0.040624 11.00000 0.09479 0.07270 = 0.05590 0.00210 -0.00971 0.03860 O2 3 0.427636 0.687303 0.040123 11.00000 0.07150 0.08393 = 0.06196 0.00729 -0.01088 0.02821 O3 3 0.333333 0.666667 0.000000 10.16667 0.04957 0.04957 = 0.01006 0.00000 0.00000 0.02478 O4 3 0.485465 0.780724 0.000000 10.50000 0.06189 0.06742 = 0.04889 0.00000 0.00000 0.02833 C1 1 0.407343 0.641526 0.053816 11.00000 0.05880 0.06042 = 0.03057 -0.00396 -0.00179 0.02648 C2 1 0.433223 0.632880 0.085400 11.00000 0.05716 0.05489 = 0.02961 0.00499 -0.00186 0.02259 C3 1 0.475627 0.672590 0.102392 11.00000 0.12404 0.10343 = 0.09902 0.02575 -0.02100 0.04857 AFIX 43 H3 2 0.488883 0.708128 0.093644 11.00000 -1.20000 AFIX 0 C4 1 0.501640 0.663824 0.132958 11.00000 0.10899 0.09900 = 0.09813 -0.00082 -0.03225 0.03215 AFIX 43 H4 2 0.531726 0.693656 0.144036 11.00000 -1.20000 AFIX 0 C5 1 0.485594 0.615670 0.146629 11.00000 0.06597 0.06783 = 0.03633 0.00440 -0.00758 0.02964 C6 1 0.443732 0.575371 0.128769 11.00000 0.13320 0.10737 = 0.11643 0.01962 -0.03238 0.04620 AFIX 43 H6 2 0.432516 0.539434 0.135539 11.00000 -1.20000 AFIX 0 C7 1 0.417355 0.585300 0.101280 11.00000 0.11356 0.11073 = 0.12049 0.00785 -0.03563 0.02838 AFIX 43 H7 2 0.384772 0.555911 0.092537 11.00000 -1.20000 AFIX 0 C8 1 0.512735 0.606222 0.177675 11.00000 0.06373 0.06909 = 0.04432 -0.00372 -0.00478 0.03120 C9 1 0.564108 0.645437 0.187455 11.00000 0.09473 0.07584 = 0.06440 0.01196 -0.00405 0.03911 AFIX 43 H9 2 0.580374 0.678811 0.174662 11.00000 -1.20000 AFIX 0 C10 1 0.592103 0.636698 0.215614 11.00000 0.07587 0.10273 = 0.07293 0.00526 -0.01262 0.03667 AFIX 43 H10 2 0.627805 0.663640 0.221064 11.00000 -1.20000 AFIX 0 C11 1 0.568683 0.588754 0.236248 11.00000 0.06875 0.06136 = 0.04086 0.00864 -0.00470 0.03009 C12 1 0.517299 0.549569 0.226490 11.00000 0.05832 0.06919 = 0.03023 -0.00043 -0.00292 0.03403 C13 1 0.490026 0.557857 0.198394 11.00000 0.05184 0.05605 = 0.04598 -0.00261 -0.00150 0.01980 AFIX 43 H13 2 0.454725 0.530340 0.192554 11.00000 -1.20000 AFIX 0 C14 1 0.500000 0.500000 0.250000 10.25000 0.06219 0.06219 = 0.02457 0.00000 0.00000 0.04127 HKLF 4 REM p in P6/mcc #192 REM R1 = 0.0547 for 2712 Fo > 4sig(Fo) and 0.0641 for all 3722 data REM 153 parameters refined using 0 restraints END WGHT 0.1062 0.0000 REM Highest difference peak 0.249, deepest hole -0.259, 1-sigma level 0.031 Q1 1 0.3978 0.6279 0.0000 10.50000 0.05 0.25 Q2 1 0.3989 0.6504 0.0000 10.50000 0.05 0.25 Q3 1 0.3238 0.6010 0.0544 11.00000 0.05 0.25 Q4 1 0.5088 0.7989 -0.0202 11.00000 0.05 0.22 Q5 1 0.4236 0.6642 0.0000 10.50000 0.05 0.22 Q6 1 0.3403 0.5878 0.0210 11.00000 0.05 0.21 Q7 1 0.3970 0.7268 0.0132 11.00000 0.05 0.19 Q8 1 0.3712 0.6984 0.0207 11.00000 0.05 0.19 Q9 1 0.4274 0.5878 0.1588 11.00000 0.05 0.19 Q10 1 0.4193 0.7076 0.0215 11.00000 0.05 0.18 Q11 1 0.3597 0.6902 0.0141 11.00000 0.05 0.18 Q12 1 0.3995 0.6879 0.0283 11.00000 0.05 0.18 Q13 1 0.3957 0.6047 0.0000 10.50000 0.05 0.17 Q14 1 0.3683 0.5981 0.0230 11.00000 0.05 0.17 Q15 1 0.4925 0.8198 0.0000 10.50000 0.05 0.17 Q16 1 0.5000 0.5000 0.1963 10.50000 0.05 0.16 Q17 1 0.4264 0.6762 0.0963 11.00000 0.05 0.15 Q18 1 0.4122 0.6748 0.0286 11.00000 0.05 0.14 Q19 1 0.5341 0.5949 0.2564 11.00000 0.05 0.13 Q20 1 0.4855 0.6660 0.0639 11.00000 0.05 0.13 ; _shelx_res_checksum 99785 _shelx_hkl_file ; ; _shelx_hkl_checksum 74205 # start Validation Reply Form _vrf_THETM01_PCN-168-100K ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The limited quality of the crystals gives rise to the weak diffraction at high angle, leading to the relatively low data completeness ; _vrf_PLAT132_PCN-168-100K ; PROBLEM: Trigonal/Hexagonal a and b Differ .............. Please Check RESPONSE: a and b are equal. ; # end Validation Reply Form ##################################################################### data_PCN-168-150K _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H32.67 Fe2 O10.67' _chemical_formula_weight 951.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 192 _space_group_name_H-M_alt 'P 6/m c c' _space_group_name_Hall '-P 6 2c' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 28.8433(9) _cell_length_b 28.843 _cell_length_c 35.7152(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 25732.0(19) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9940 _cell_measurement_theta_min 2.4742 _cell_measurement_theta_max 43.0238 _exptl_crystal_description Rod-like _exptl_crystal_colour Dark-red _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 0.369 _exptl_crystal_F_000 2928 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 1.493 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.3036 _exptl_absorpt_correction_T_max 0.7485 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3220 _diffrn_reflns_av_unetI/netI 0.0641 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.474 _diffrn_reflns_theta_max 43.235 _diffrn_reflns_theta_full 43.235 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_point_group_measured_fraction_full 0.991 _reflns_number_total 3220 _reflns_number_gt 1984 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _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. ; _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2014)' _computing_publication_material 'SHELXTL (Sheldrick, 2014)' _refine_special_details ; ? ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.004 -0.006 -0.004 21052 8003 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1142P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3220 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1676 _refine_ls_wR_factor_gt 0.1594 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _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_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 0.72153(3) 0.40693(3) 0.0000 0.0666(5) Uani 1 2 d S T P . . O1 O 0.76456(13) 0.39788(13) 0.04006(10) 0.0967(12) Uani 1 1 d . . . . . O2 O 0.74064(14) 0.31273(15) 0.03988(10) 0.0957(12) Uani 1 1 d . . . . . O3 O 0.6667 0.3333 0.0000 0.084(2) Uani 1 6 d S T P . . O4 O 0.78122(14) 0.48623(14) 0.0000 0.0846(13) Uani 1 2 d S T P . . C1 C 0.7661(2) 0.3585(3) 0.05357(17) 0.0753(15) Uani 1 1 d . . . . . C2 C 0.8007(2) 0.3675(3) 0.08514(17) 0.0672(13) Uani 1 1 d . . . . . C3 C 0.8040(3) 0.3277(3) 0.1022(2) 0.126(2) Uani 1 1 d . . . . . H3 H 0.7820 0.2922 0.0932 0.151 Uiso 1 1 calc R U . . . C4 C 0.8380(3) 0.3354(3) 0.1324(3) 0.144(3) Uani 1 1 d . . . . . H4 H 0.8381 0.3053 0.1430 0.172 Uiso 1 1 calc R U . . . C5 C 0.8701(2) 0.3837(4) 0.14681(18) 0.0843(17) Uani 1 1 d . . . . . C6 C 0.8674(3) 0.4238(3) 0.1299(2) 0.147(3) Uani 1 1 d . . . . . H6 H 0.8916 0.4594 0.1377 0.176 Uiso 1 1 calc R U . . . C7 C 0.8324(4) 0.4160(3) 0.1027(2) 0.145(2) Uani 1 1 d . . . . . H7 H 0.8291 0.4457 0.0949 0.174 Uiso 1 1 calc R U . . . C8 C 0.9066(2) 0.3945(3) 0.17732(19) 0.0840(16) Uani 1 1 d . . . . . C9 C 0.9177(2) 0.3543(2) 0.18749(17) 0.0989(17) Uani 1 1 d . . . . . H9 H 0.8995 0.3206 0.1752 0.119 Uiso 1 1 calc R U . . . C10 C 0.9542(3) 0.3627(2) 0.21478(19) 0.1052(17) Uani 1 1 d . . . . . H10 H 0.9626 0.3354 0.2198 0.126 Uiso 1 1 calc R U . . . C11 C 0.98005(17) 0.4107(3) 0.23588(12) 0.0768(14) Uani 1 1 d . . . . . C12 C 0.96821(19) 0.45077(19) 0.22658(14) 0.0714(14) Uani 1 1 d . . . . . C13 C 0.9322(2) 0.4429(2) 0.19846(17) 0.0717(14) Uani 1 1 d . . . . . H13 H 0.9243 0.4704 0.1930 0.086 Uiso 1 1 calc R U . . . C14 C 1.0000 0.5000 0.2500 0.058(2) Uani 1 4 d S T P . . 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 0.0766(8) 0.0816(8) 0.0436(8) 0.000 0.000 0.0410(6) O1 0.112(3) 0.096(3) 0.079(3) -0.005(2) -0.012(2) 0.050(2) O2 0.123(3) 0.106(3) 0.068(3) -0.012(2) -0.022(2) 0.065(2) O3 0.091(3) 0.091(3) 0.070(5) 0.000 0.000 0.0457(15) O4 0.097(3) 0.075(3) 0.070(3) 0.000 0.000 0.034(2) C1 0.096(4) 0.112(6) 0.030(4) -0.016(4) -0.013(4) 0.061(4) C2 0.085(4) 0.078(4) 0.036(4) -0.002(4) -0.001(4) 0.039(4) C3 0.140(6) 0.124(6) 0.101(6) -0.004(5) -0.036(5) 0.056(5) C4 0.163(6) 0.132(7) 0.129(7) -0.034(5) -0.047(5) 0.069(6) C5 0.103(4) 0.132(6) 0.041(5) 0.004(5) -0.025(4) 0.076(5) C6 0.172(7) 0.185(8) 0.092(6) -0.015(6) -0.062(5) 0.095(6) C7 0.186(6) 0.133(7) 0.114(6) -0.026(6) -0.041(5) 0.079(6) C8 0.103(4) 0.096(5) 0.061(5) 0.022(5) 0.011(4) 0.056(4) C9 0.106(4) 0.114(5) 0.064(5) 0.001(4) -0.016(4) 0.046(4) C10 0.127(5) 0.124(6) 0.078(5) -0.022(4) -0.017(4) 0.073(4) C11 0.093(4) 0.090(4) 0.046(5) -0.003(3) -0.012(3) 0.044(4) C12 0.081(4) 0.108(5) 0.032(4) 0.001(3) -0.008(4) 0.053(3) C13 0.089(4) 0.073(4) 0.052(4) -0.003(3) 0.004(3) 0.040(3) C14 0.056(6) 0.097(6) 0.009(7) 0.000 0.000 0.028(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 O3 1.9108(9) . ? Fe1 O2 1.992(4) 18_655 ? Fe1 O2 1.992(4) 3_655 ? Fe1 O1 1.995(4) 16 ? Fe1 O1 1.995(4) . ? Fe1 O4 2.063(4) . ? O1 C1 1.257(5) . ? O2 C1 1.245(5) . ? O2 Fe1 1.992(4) 14_665 ? O3 Fe1 1.9108(9) 14_665 ? O3 Fe1 1.9108(9) 3_655 ? C1 C2 1.440(6) . ? C2 C3 1.345(6) . ? C2 C7 1.379(7) . ? C3 C4 1.398(7) . ? C4 C5 1.330(7) . ? C5 C6 1.340(7) . ? C5 C8 1.436(6) . ? C6 C7 1.340(7) . ? C8 C9 1.396(6) . ? C8 C13 1.426(6) . ? C9 C10 1.365(6) . ? C10 C11 1.417(5) . ? C11 C12 1.399(5) . ? C11 C11 1.418(9) 8_765 ? C12 C13 1.379(5) . ? C12 C14 1.502(5) . ? C14 C12 1.502(5) 4_765 ? C14 C12 1.502(5) 8_765 ? C14 C12 1.502(5) 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 O3 Fe1 O2 94.38(10) . 18_655 ? O3 Fe1 O2 94.38(10) . 3_655 ? O2 Fe1 O2 91.26(19) 18_655 3_655 ? O3 Fe1 O1 94.51(10) . 16 ? O2 Fe1 O1 87.85(13) 18_655 16 ? O2 Fe1 O1 171.11(13) 3_655 16 ? O3 Fe1 O1 94.51(10) . . ? O2 Fe1 O1 171.11(13) 18_655 . ? O2 Fe1 O1 87.85(13) 3_655 . ? O1 Fe1 O1 91.66(19) 16 . ? O3 Fe1 O4 179.56(11) . . ? O2 Fe1 O4 85.92(12) 18_655 . ? O2 Fe1 O4 85.92(12) 3_655 . ? O1 Fe1 O4 85.19(12) 16 . ? O1 Fe1 O4 85.19(12) . . ? C1 O1 Fe1 134.4(4) . . ? C1 O2 Fe1 135.1(4) . 14_665 ? Fe1 O3 Fe1 119.999(1) 14_665 . ? Fe1 O3 Fe1 120.000(1) 14_665 3_655 ? Fe1 O3 Fe1 120.001(1) . 3_655 ? O2 C1 O1 122.6(6) . . ? O2 C1 C2 119.2(6) . . ? O1 C1 C2 118.1(6) . . ? C3 C2 C7 111.5(6) . . ? C3 C2 C1 122.5(7) . . ? C7 C2 C1 125.9(7) . . ? C2 C3 C4 123.8(6) . . ? C5 C4 C3 122.2(6) . . ? C4 C5 C6 114.7(6) . . ? C4 C5 C8 124.9(8) . . ? C6 C5 C8 120.4(8) . . ? C5 C6 C7 123.2(7) . . ? C6 C7 C2 124.1(7) . . ? C9 C8 C13 116.9(6) . . ? C9 C8 C5 117.7(7) . . ? C13 C8 C5 125.4(7) . . ? C10 C9 C8 121.1(6) . . ? C9 C10 C11 122.3(5) . . ? C12 C11 C11 108.5(3) . 8_765 ? C12 C11 C10 117.0(4) . . ? C11 C11 C10 134.3(4) 8_765 . ? C13 C12 C11 120.8(4) . . ? C13 C12 C14 128.0(5) . . ? C11 C12 C14 111.3(5) . . ? C12 C13 C8 121.8(5) . . ? C12 C14 C12 112.3(4) . 4_765 ? C12 C14 C12 100.4(5) . 8_765 ? C12 C14 C12 116.1(4) 4_765 8_765 ? C12 C14 C12 116.1(4) . 12 ? C12 C14 C12 100.4(5) 4_765 12 ? C12 C14 C12 112.3(4) 8_765 12 ? _refine_diff_density_max 0.251 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.028 _shelx_res_file ; C:\PCN-168\150K\PCN-168-150K.res created by SHELXL-2014/7 REM reset to P6/mcc #192 REM REM REM REM p in P6/mcc #192 REM R1 = 0.3693 for 2268 Fo > 4sig(Fo) and 0.4127 for all 3220 data REM 69 parameters refined using 0 restraints REM Highest difference peak 3.012, deepest hole -2.127, 1-sigma level 0.215 REM p in P6/mcc #192 REM R1 = 0.3739 for 2268 Fo > 4sig(Fo) and 0.4145 for all 3220 data REM 69 parameters refined using 0 restraints REM Highest difference peak 3.012, deepest hole -2.150, 1-sigma level 0.219 TITL p in P6/mcc #192 CELL 1.54184 28.8433 28.8433 35.7152 90.000 90.000 120.000 ZERR 6.0000 0.0009 0.0000 0.0015 0.000 0.000 0.000 LATT 1 SYMM X-Y, X, Z SYMM -Y, X-Y, Z SYMM -X, -Y, Z SYMM -X+Y, -X, Z SYMM Y, -X+Y, Z SYMM X-Y, -Y, 0.5-Z SYMM -X, -X+Y, 0.5-Z SYMM Y, X, 0.5-Z SYMM -Y, -X, 0.5-Z SYMM -X+Y, Y, 0.5-Z SYMM X, X-Y, 0.5-Z SFAC C H O FE UNIT 318 196.0002 64.0002 12 MERG 2 FMAP 2 GRID PLAN 20 TEMP -123 BOND L.S. 20 ACTA WGHT 0.114200 FVAR 1.90550 FE1 4 0.721535 0.406927 0.000000 10.50000 0.07656 0.08158 = 0.04364 0.00000 0.00000 0.04103 O1 3 0.764558 0.397883 0.040063 11.00000 0.11240 0.09595 = 0.07897 -0.00521 -0.01205 0.04990 O2 3 0.740639 0.312726 0.039879 11.00000 0.12308 0.10627 = 0.06799 -0.01197 -0.02166 0.06493 O3 3 0.666667 0.333333 0.000000 10.16667 0.09145 0.09145 = 0.06951 0.00000 0.00000 0.04572 O4 3 0.781224 0.486229 0.000000 10.50000 0.09670 0.07497 = 0.06956 0.00000 0.00000 0.03357 C1 1 0.766144 0.358458 0.053568 11.00000 0.09620 0.11179 = 0.02980 -0.01626 -0.01286 0.06094 C2 1 0.800740 0.367520 0.085138 11.00000 0.08542 0.07822 = 0.03585 -0.00177 -0.00140 0.03939 C3 1 0.804029 0.327683 0.102194 11.00000 0.13972 0.12430 = 0.10060 -0.00443 -0.03648 0.05612 AFIX 43 H3 2 0.782007 0.292238 0.093197 11.00000 -1.20000 AFIX 0 C4 1 0.837994 0.335450 0.132397 11.00000 0.16263 0.13212 = 0.12931 -0.03419 -0.04722 0.06885 AFIX 43 H4 2 0.838140 0.305302 0.142974 11.00000 -1.20000 AFIX 0 C5 1 0.870114 0.383669 0.146810 11.00000 0.10305 0.13178 = 0.04081 0.00420 -0.02508 0.07587 C6 1 0.867448 0.423756 0.129923 11.00000 0.17243 0.18470 = 0.09168 -0.01473 -0.06221 0.09512 AFIX 43 H6 2 0.891582 0.459407 0.137659 11.00000 -1.20000 AFIX 0 C7 1 0.832381 0.415971 0.102651 11.00000 0.18622 0.13343 = 0.11416 -0.02558 -0.04065 0.07921 AFIX 43 H7 2 0.829106 0.445709 0.094888 11.00000 -1.20000 AFIX 0 C8 1 0.906564 0.394497 0.177318 11.00000 0.10340 0.09604 = 0.06105 0.02166 0.01147 0.05619 C9 1 0.917685 0.354336 0.187494 11.00000 0.10594 0.11449 = 0.06367 0.00095 -0.01615 0.04575 AFIX 43 H9 2 0.899535 0.320619 0.175232 11.00000 -1.20000 AFIX 0 C10 1 0.954221 0.362718 0.214782 11.00000 0.12741 0.12383 = 0.07770 -0.02225 -0.01651 0.07270 AFIX 43 H10 2 0.962622 0.335403 0.219802 11.00000 -1.20000 AFIX 0 C11 1 0.980051 0.410705 0.235879 11.00000 0.09289 0.08958 = 0.04589 -0.00264 -0.01165 0.04412 C12 1 0.968205 0.450769 0.226578 11.00000 0.08146 0.10791 = 0.03224 0.00129 -0.00827 0.05295 C13 1 0.932203 0.442884 0.198460 11.00000 0.08933 0.07256 = 0.05230 -0.00313 0.00369 0.03979 AFIX 43 H13 2 0.924277 0.470428 0.193036 11.00000 -1.20000 AFIX 0 C14 1 1.000000 0.500000 0.250000 10.25000 0.05576 0.09659 = 0.00853 0.00000 0.00000 0.02788 HKLF 4 REM p in P6/mcc #192 REM R1 = 0.0612 for 1984 Fo > 4sig(Fo) and 0.0812 for all 3220 data REM 153 parameters refined using 0 restraints END WGHT 0.1137 0.0000 REM Highest difference peak 0.251, deepest hole -0.376, 1-sigma level 0.028 Q1 1 0.7623 0.3518 0.0000 10.50000 0.05 0.25 Q2 1 0.7669 0.3331 0.0000 10.50000 0.05 0.23 Q3 1 0.7306 0.4022 0.0608 11.00000 0.05 0.22 Q4 1 0.8388 0.4018 0.1615 11.00000 0.05 0.20 Q5 1 0.8298 0.5009 0.0000 10.50000 0.05 0.19 Q6 1 0.7807 0.4066 0.0295 11.00000 0.05 0.18 Q7 1 0.9001 0.4906 0.1303 11.00000 0.05 0.18 Q8 1 0.6910 0.3911 -0.0245 11.00000 0.05 0.18 Q9 1 0.7475 0.4261 0.0649 11.00000 0.05 0.17 Q10 1 0.7611 0.4113 0.0279 11.00000 0.05 0.16 Q11 1 0.8096 0.4968 -0.0195 11.00000 0.05 0.14 Q12 1 0.7584 0.3392 0.1032 11.00000 0.05 0.14 Q13 1 0.8489 0.4289 0.1685 11.00000 0.05 0.14 Q14 1 0.7116 0.3007 0.0222 11.00000 0.05 0.14 Q15 1 0.8189 0.5276 0.0000 10.50000 0.05 0.13 Q16 1 0.7964 0.3974 0.0000 10.50000 0.05 0.13 Q17 1 0.9180 0.4369 0.1383 11.00000 0.05 0.13 Q18 1 0.8198 0.3479 0.0625 11.00000 0.05 0.13 Q19 1 0.7907 0.5092 0.0199 11.00000 0.05 0.13 Q20 1 0.7957 0.4643 -0.0272 11.00000 0.05 0.12 ; _shelx_res_checksum 46435 _shelx_hkl_file ; ; _shelx_hkl_checksum 39640 # start Validation Reply Form _vrf_THETM01_PCN-168-150K ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The limited quality of the crystals gives rise to the weak diffraction at hgih angle, leading to the relatively low data completeness ; _vrf_PLAT132_PCN-168-150K ; PROBLEM: Trigonal/Hexagonal a and b Differ .............. Please Check RESPONSE: a and b are equal. ; # end Validation Reply Form ##################################################################### data_PCN-168-200K _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H32.67 Fe2 O10.67' _chemical_formula_weight 951.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 192 _space_group_name_H-M_alt 'P 6/m c c' _space_group_name_Hall '-P 6 2c' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 31.4730(7) _cell_length_b 31.473 _cell_length_c 33.1372(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 28426.4(15) _cell_formula_units_Z 6 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9920 _cell_measurement_theta_min 2.6669 _cell_measurement_theta_max 43.6998 _exptl_crystal_description Rod-like _exptl_crystal_colour Dark-red _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 0.334 _exptl_crystal_F_000 2928 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 1.351 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.3017 _exptl_absorpt_correction_T_max 0.7486 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3676 _diffrn_reflns_av_unetI/netI 0.0513 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.667 _diffrn_reflns_theta_max 43.752 _diffrn_reflns_theta_full 43.752 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 3676 _reflns_number_gt 2896 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _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. ; _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2014)' _computing_publication_material 'SHELXTL (Sheldrick, 2014)' _refine_special_details ; ? ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.003 -0.005 -0.004 23995 10133 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1010P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3676 _refine_ls_number_parameters 153 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1432 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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_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 0.28426(2) 0.59861(2) 0.0000 0.0158(3) Uani 1 2 d S T P . . O1 O 0.39506(8) 0.63786(9) 0.04313(6) 0.0328(7) Uani 1 1 d . . . . . O2 O 0.31666(9) 0.57988(8) 0.04321(7) 0.0372(7) Uani 1 1 d . . . . . O3 O 0.3333 0.6667 0.0000 0.0152(12) Uani 1 6 d S T P . . O4 O 0.23220(10) 0.52593(10) 0.0000 0.0386(9) Uani 1 2 d S T P . . C1 C 0.35999(15) 0.59844(13) 0.05589(11) 0.0194(9) Uani 1 1 d . . . . . C2 C 0.37005(14) 0.57249(13) 0.08748(10) 0.0192(9) Uani 1 1 d . . . . . C3 C 0.33406(17) 0.53187(19) 0.10463(14) 0.0750(14) Uani 1 1 d . . . . . H3 H 0.3011 0.5208 0.0969 0.090 Uiso 1 1 calc R U . . . C4 C 0.34351(18) 0.50484(16) 0.13400(14) 0.0880(15) Uani 1 1 d . . . . . H4 H 0.3169 0.4760 0.1452 0.106 Uiso 1 1 calc R U . . . C5 C 0.39034(14) 0.51953(14) 0.14660(10) 0.0285(9) Uani 1 1 d . . . . . C6 C 0.42586(16) 0.56098(18) 0.12976(15) 0.0717(13) Uani 1 1 d . . . . . H6 H 0.4590 0.5734 0.1379 0.086 Uiso 1 1 calc R U . . . C7 C 0.41492(19) 0.58622(15) 0.10040(14) 0.0714(13) Uani 1 1 d . . . . . H7 H 0.4414 0.6150 0.0891 0.086 Uiso 1 1 calc R U . . . C8 C 0.40004(12) 0.49131(13) 0.17736(10) 0.0286(9) Uani 1 1 d . . . . . C9 C 0.36480(13) 0.44413(15) 0.18651(11) 0.0474(11) Uani 1 1 d . . . . . H9 H 0.3341 0.4297 0.1730 0.057 Uiso 1 1 calc R U . . . C10 C 0.37332(14) 0.41702(13) 0.21513(12) 0.0521(11) Uani 1 1 d . . . . . H10 H 0.3485 0.3845 0.2214 0.062 Uiso 1 1 calc R U . . . C11 C 0.41929(13) 0.43830(12) 0.23494(9) 0.0305(9) Uani 1 1 d . . . . . C12 C 0.45433(10) 0.48525(11) 0.22546(9) 0.0191(8) Uani 1 1 d . . . . . C13 C 0.44542(11) 0.51166(11) 0.19698(10) 0.0211(8) Uani 1 1 d . U . . . H13 H 0.4704 0.5441 0.1906 0.025 Uiso 1 1 calc R U . . . C14 C 0.5000 0.5000 0.2500 0.0136(15) Uani 1 4 d S T P . . 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 0.0203(5) 0.0213(5) 0.0074(6) 0.000 0.000 0.0115(4) O1 0.0354(15) 0.0427(16) 0.0196(19) 0.0096(12) -0.0004(12) 0.0190(14) O2 0.0380(17) 0.0382(15) 0.031(2) 0.0089(12) -0.0078(13) 0.0155(13) O3 0.0218(17) 0.0218(17) 0.002(3) 0.000 0.000 0.0109(8) O4 0.043(2) 0.043(2) 0.029(2) 0.000 0.000 0.0212(17) C1 0.031(3) 0.025(2) 0.005(2) 0.001(2) 0.006(2) 0.017(2) C2 0.016(2) 0.024(2) 0.011(3) 0.005(2) -0.002(2) 0.004(2) C3 0.057(3) 0.085(4) 0.081(4) 0.017(3) -0.023(3) 0.033(3) C4 0.065(4) 0.074(3) 0.099(4) 0.037(3) -0.004(3) 0.016(3) C5 0.031(3) 0.036(3) 0.018(3) 0.005(2) 0.001(2) 0.016(2) C6 0.049(3) 0.076(4) 0.078(4) 0.018(3) -0.011(3) 0.022(3) C7 0.066(4) 0.058(3) 0.068(4) 0.026(3) 0.003(3) 0.014(3) C8 0.030(2) 0.034(3) 0.020(3) 0.000(2) -0.005(2) 0.015(2) C9 0.040(3) 0.055(3) 0.042(3) 0.005(2) -0.012(2) 0.019(3) C10 0.058(3) 0.044(2) 0.049(3) 0.017(2) -0.004(2) 0.021(2) C11 0.034(2) 0.039(2) 0.020(3) 0.0016(18) -0.0043(19) 0.0192(19) C12 0.027(2) 0.020(2) 0.010(2) -0.0004(18) 0.0030(17) 0.011(2) C13 0.026(2) 0.0203(18) 0.012(2) 0.0059(18) 0.0047(17) 0.0073(16) C14 0.019(3) 0.019(3) 0.004(4) 0.000 0.000 0.011(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 O3 1.9145(6) . ? Fe1 O2 2.010(2) . ? Fe1 O2 2.010(2) 16 ? Fe1 O1 2.011(2) 14_565 ? Fe1 O1 2.011(2) 5_565 ? Fe1 O4 2.042(3) . ? O1 C1 1.252(3) . ? O1 Fe1 2.011(2) 3_665 ? O2 C1 1.257(4) . ? O3 Fe1 1.9147(6) 14_565 ? O3 Fe1 1.9145(6) 3_665 ? C1 C2 1.457(4) . ? C2 C7 1.325(5) . ? C2 C3 1.339(5) . ? C3 C4 1.419(5) . ? C4 C5 1.371(5) . ? C5 C6 1.343(5) . ? C5 C8 1.480(4) . ? C6 C7 1.404(5) . ? C8 C9 1.371(4) . ? C8 C13 1.399(4) . ? C9 C10 1.389(4) . ? C10 C11 1.415(4) . ? C11 C12 1.367(4) . ? C11 C11 1.439(6) 9 ? C12 C13 1.376(4) . ? C12 C14 1.508(3) . ? C14 C12 1.508(3) 10_665 ? C14 C12 1.508(3) 4_665 ? C14 C12 1.508(3) 9 ? 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 O3 Fe1 O2 94.84(7) . . ? O3 Fe1 O2 94.84(7) . 16 ? O2 Fe1 O2 90.89(13) . 16 ? O3 Fe1 O1 95.13(7) . 14_565 ? O2 Fe1 O1 170.03(9) . 14_565 ? O2 Fe1 O1 88.41(9) 16 14_565 ? O3 Fe1 O1 95.13(7) . 5_565 ? O2 Fe1 O1 88.42(9) . 5_565 ? O2 Fe1 O1 170.03(9) 16 5_565 ? O1 Fe1 O1 90.55(12) 14_565 5_565 ? O3 Fe1 O4 179.72(9) . . ? O2 Fe1 O4 84.96(9) . . ? O2 Fe1 O4 84.96(9) 16 . ? O1 Fe1 O4 85.07(9) 14_565 . ? O1 Fe1 O4 85.07(9) 5_565 . ? C1 O1 Fe1 133.6(2) . 3_665 ? C1 O2 Fe1 133.9(2) . . ? Fe1 O3 Fe1 119.998(1) 14_565 . ? Fe1 O3 Fe1 119.998(1) 14_565 3_665 ? Fe1 O3 Fe1 120.003(1) . 3_665 ? O1 C1 O2 124.2(3) . . ? O1 C1 C2 117.9(3) . . ? O2 C1 C2 118.0(3) . . ? C7 C2 C3 115.4(3) . . ? C7 C2 C1 123.0(4) . . ? C3 C2 C1 121.5(4) . . ? C2 C3 C4 122.2(4) . . ? C5 C4 C3 121.3(4) . . ? C6 C5 C4 115.7(3) . . ? C6 C5 C8 123.2(4) . . ? C4 C5 C8 121.1(4) . . ? C5 C6 C7 121.1(4) . . ? C2 C7 C6 124.3(4) . . ? C9 C8 C13 118.7(3) . . ? C9 C8 C5 120.3(3) . . ? C13 C8 C5 121.0(3) . . ? C8 C9 C10 121.1(3) . . ? C9 C10 C11 119.5(3) . . ? C12 C11 C10 119.1(3) . . ? C12 C11 C11 109.29(19) . 9 ? C10 C11 C11 131.6(2) . 9 ? C11 C12 C13 120.8(3) . . ? C11 C12 C14 109.8(3) . . ? C13 C12 C14 129.4(3) . . ? C12 C13 C8 120.8(3) . . ? C12 C14 C12 101.9(3) 10_665 4_665 ? C12 C14 C12 114.8(2) 10_665 9 ? C12 C14 C12 112.1(2) 4_665 9 ? C12 C14 C12 112.1(2) 10_665 . ? C12 C14 C12 114.8(2) 4_665 . ? C12 C14 C12 101.9(3) 9 . ? _refine_diff_density_max 0.260 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.034 _shelx_res_file ; C:\PCN-168\200K\PCN-168-200K.res created by SHELXL-2014/7 REM reset to P6/mcc #192 REM REM REM REM p in P6/mcc #192 REM R1 = 0.2787 for 3075 Fo > 4sig(Fo) and 0.2924 for all 3676 data REM 69 parameters refined using 0 restraints REM Highest difference peak 2.465, deepest hole -1.922, 1-sigma level 0.213 REM p in P6/mcc #192 REM R1 = 0.2787 for 3075 Fo > 4sig(Fo) and 0.2924 for all 3676 data REM 69 parameters refined using 0 restraints REM Highest difference peak 2.465, deepest hole -1.922, 1-sigma level 0.213 TITL p in P6/mcc #192 CELL 1.54184 31.4730 31.4730 33.1372 90.000 90.000 120.000 ZERR 6.0000 0.0007 0.0000 0.0010 0.000 0.000 0.000 LATT 1 SYMM X-Y, X, Z SYMM -Y, X-Y, Z SYMM -X, -Y, Z SYMM -X+Y, -X, Z SYMM Y, -X+Y, Z SYMM X-Y, -Y, 0.5-Z SYMM -X, -X+Y, 0.5-Z SYMM Y, X, 0.5-Z SYMM -Y, -X, 0.5-Z SYMM -X+Y, Y, 0.5-Z SYMM X, X-Y, 0.5-Z SFAC C H O FE UNIT 318 196.0002 64.0002 12 MERG 2 FMAP 2 GRID PLAN 20 TEMP -73 BOND ISOR 0.005 C13 L.S. 20 ACTA WGHT 0.101000 FVAR 1.50148 FE1 4 0.284263 0.598605 0.000000 10.50000 0.02028 0.02132 = 0.00740 0.00000 0.00000 0.01153 O1 3 0.395057 0.637856 0.043127 11.00000 0.03536 0.04269 = 0.01956 0.00959 -0.00038 0.01902 O2 3 0.316663 0.579884 0.043212 11.00000 0.03797 0.03823 = 0.03051 0.00891 -0.00785 0.01546 O3 3 0.333333 0.666667 0.000000 10.16667 0.02181 0.02181 = 0.00185 0.00000 0.00000 0.01091 O4 3 0.232199 0.525929 0.000000 10.50000 0.04316 0.04296 = 0.02931 0.00000 0.00000 0.02121 C1 1 0.359988 0.598440 0.055889 11.00000 0.03125 0.02529 = 0.00526 0.00095 0.00624 0.01685 C2 1 0.370052 0.572492 0.087479 11.00000 0.01577 0.02368 = 0.01097 0.00502 -0.00209 0.00447 C3 1 0.334064 0.531874 0.104627 11.00000 0.05658 0.08459 = 0.08096 0.01727 -0.02302 0.03312 AFIX 43 H3 2 0.301094 0.520780 0.096864 11.00000 -1.20000 AFIX 0 C4 1 0.343506 0.504841 0.134003 11.00000 0.06482 0.07427 = 0.09910 0.03664 -0.00414 0.01551 AFIX 43 H4 2 0.316859 0.476004 0.145158 11.00000 -1.20000 AFIX 0 C5 1 0.390340 0.519527 0.146603 11.00000 0.03073 0.03576 = 0.01767 0.00467 0.00050 0.01570 C6 1 0.425865 0.560976 0.129763 11.00000 0.04869 0.07565 = 0.07810 0.01816 -0.01131 0.02165 AFIX 43 H6 2 0.458959 0.573415 0.137867 11.00000 -1.20000 AFIX 0 C7 1 0.414923 0.586219 0.100403 11.00000 0.06589 0.05763 = 0.06777 0.02559 0.00325 0.01362 AFIX 43 H7 2 0.441423 0.615022 0.089063 11.00000 -1.20000 AFIX 0 C8 1 0.400045 0.491313 0.177359 11.00000 0.03013 0.03398 = 0.01973 -0.00038 -0.00450 0.01463 C9 1 0.364802 0.444128 0.186510 11.00000 0.03983 0.05455 = 0.04202 0.00463 -0.01237 0.01933 AFIX 43 H9 2 0.334052 0.429747 0.173046 11.00000 -1.20000 AFIX 0 C10 1 0.373325 0.417020 0.215135 11.00000 0.05780 0.04356 = 0.04863 0.01706 -0.00430 0.02066 AFIX 43 H10 2 0.348507 0.384461 0.221374 11.00000 -1.20000 AFIX 0 C11 1 0.419288 0.438300 0.234937 11.00000 0.03424 0.03882 = 0.01951 0.00165 -0.00431 0.01918 C12 1 0.454328 0.485250 0.225465 11.00000 0.02654 0.01996 = 0.00951 -0.00039 0.00302 0.01064 C13 1 0.445420 0.511656 0.196980 11.00000 0.02573 0.02028 = 0.01181 0.00593 0.00473 0.00729 AFIX 43 H13 2 0.470378 0.544090 0.190557 11.00000 -1.20000 AFIX 0 C14 1 0.500000 0.500000 0.250000 10.25000 0.01894 0.01894 = 0.00434 0.00000 0.00000 0.01056 HKLF 4 REM p in P6/mcc #192 REM R1 = 0.0521 for 2896 Fo > 4sig(Fo) and 0.0609 for all 3676 data REM 153 parameters refined using 6 restraints END WGHT 0.1010 0.0000 REM Highest difference peak 0.260, deepest hole -0.345, 1-sigma level 0.034 Q1 1 0.2841 0.6013 0.0379 11.00000 0.05 0.23 Q2 1 0.2027 0.5126 0.0000 10.50000 0.05 0.23 Q3 1 0.2523 0.5085 0.0000 10.50000 0.05 0.23 Q4 1 0.2206 0.5105 0.0385 11.00000 0.05 0.22 Q5 1 0.4150 0.5860 0.1511 11.00000 0.05 0.21 Q6 1 0.4280 0.6659 0.0699 11.00000 0.05 0.20 Q7 1 0.4414 0.5997 0.1541 11.00000 0.05 0.20 Q8 1 0.2886 0.5263 0.0000 10.50000 0.05 0.19 Q9 1 0.5000 0.5000 0.2135 10.50000 0.05 0.19 Q10 1 0.3761 0.6112 0.0933 11.00000 0.05 0.18 Q11 1 0.3553 0.5933 0.0943 11.00000 0.05 0.18 Q12 1 0.3305 0.5096 0.0651 11.00000 0.05 0.18 Q13 1 0.4389 0.5788 0.1715 11.00000 0.05 0.17 Q14 1 0.4614 0.6178 0.1250 11.00000 0.05 0.17 Q15 1 0.4590 0.6307 0.1198 11.00000 0.05 0.16 Q16 1 0.4022 0.4980 0.2085 11.00000 0.05 0.16 Q17 1 0.4542 0.5956 0.1314 11.00000 0.05 0.15 Q18 1 0.3268 0.5972 0.0777 11.00000 0.05 0.15 Q19 1 0.3718 0.5720 0.0649 11.00000 0.05 0.15 Q20 1 0.4635 0.5184 0.2328 11.00000 0.05 0.15 ; _shelx_res_checksum 67334 _shelx_hkl_file ; ; _shelx_hkl_checksum 65470 # start Validation Reply Form _vrf_THETM01_PCN-168-200K ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The limited quality of the crystals gives rise to the weak diffraction at high angle, leading to the relatively low data completeness ; # end Validation Reply Form ##################################################################### data_PCN-168-250K _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H32.67 Fe2 O10.67' _chemical_formula_weight 951.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 192 _space_group_name_H-M_alt 'P 6/m c c' _space_group_name_Hall '-P 6 2c' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 31.3244(10) _cell_length_b 31.324 _cell_length_c 33.2713(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 28273(2) _cell_formula_units_Z 6 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 9896 _cell_measurement_theta_min 3.1162 _cell_measurement_theta_max 46.3049 _exptl_crystal_description Rod-like _exptl_crystal_colour Dark-red _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 0.335 _exptl_crystal_F_000 2928 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 1.359 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.3386 _exptl_absorpt_correction_T_max 0.7491 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4208 _diffrn_reflns_av_unetI/netI 0.0344 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.656 _diffrn_reflns_theta_max 46.412 _diffrn_reflns_theta_full 46.412 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 4208 _reflns_number_gt 3369 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _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. ; _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2014)' _computing_publication_material 'SHELXTL (Sheldrick, 2014)' _refine_special_details ; ? ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.003 -0.005 -0.004 23595 4103 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4208 _refine_ls_number_parameters 153 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 0.524 _refine_ls_restrained_S_all 0.528 _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_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 0.40166(2) 0.71604(2) 0.0000 0.0268(2) Uani 1 2 d S T P . . C14 C 0.5000 1.0000 -0.2500 0.0299(10) Uani 1 4 d S T P . . O4 O 0.47462(7) 0.76846(8) 0.0000 0.0602(6) Uani 1 2 d S T P . . O3 O 0.3333 0.6667 0.0000 0.0262(7) Uani 1 6 d S T P . . O2 O 0.39490(6) 0.75740(5) -0.04287(4) 0.0496(5) Uani 1 1 d . . . . . C10 C 0.45402(7) 0.96940(7) -0.22502(5) 0.0318(5) Uani 1 1 d . U . . . C8 C 0.39902(8) 0.90868(8) -0.17764(6) 0.0483(7) Uani 1 1 d . . . . . C2 C 0.36948(8) 0.79804(8) -0.08781(5) 0.0367(6) Uani 1 1 d . . . . . C5 C 0.39000(9) 0.87052(8) -0.14642(6) 0.0502(7) Uani 1 1 d . . . . . O1 O 0.31650(5) 0.73668(6) -0.04328(4) 0.0539(5) Uani 1 1 d . . . . . C1 C 0.35971(9) 0.76161(7) -0.05578(6) 0.0304(5) Uani 1 1 d . U . . . C11 C 0.41798(9) 0.98067(8) -0.23465(6) 0.0485(6) Uani 1 1 d . . . . . C9 C 0.44528(7) 0.93349(7) -0.19665(5) 0.0367(6) Uani 1 1 d . U . . . H9 H 0.4699 0.9259 -0.1902 0.044 Uiso 1 1 calc R U . . . C13 C 0.36409(10) 0.92145(10) -0.18690(7) 0.0738(8) Uani 1 1 d . . . . . H13 H 0.3336 0.9058 -0.1735 0.089 Uiso 1 1 calc R U . . . C3 C 0.41660(11) 0.83005(11) -0.09975(8) 0.0947(10) Uani 1 1 d . . . . . H3 H 0.4428 0.8277 -0.0883 0.114 Uiso 1 1 calc R U . . . C4 C 0.42663(10) 0.86602(11) -0.12853(9) 0.0990(11) Uani 1 1 d . . . . . H4 H 0.4595 0.8878 -0.1358 0.119 Uiso 1 1 calc R U . . . C7 C 0.33266(10) 0.80232(11) -0.10514(8) 0.0970(11) Uani 1 1 d . . . . . H7 H 0.2999 0.7808 -0.0973 0.116 Uiso 1 1 calc R U . . . C12 C 0.37280(9) 0.95666(10) -0.21540(7) 0.0748(8) Uani 1 1 d . . . . . H12 H 0.3482 0.9644 -0.2218 0.090 Uiso 1 1 calc R U . . . C6 C 0.34218(10) 0.83771(11) -0.13418(8) 0.1040(12) Uani 1 1 d . . . . . H6 H 0.3158 0.8395 -0.1458 0.125 Uiso 1 1 calc R U . . . 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 0.0399(4) 0.0383(4) 0.0055(3) 0.000 0.000 0.0219(3) C14 0.0385(18) 0.032(2) 0.017(2) 0.000 0.000 0.0159(12) O4 0.0437(14) 0.0586(15) 0.0722(14) 0.000 0.000 0.0212(12) O3 0.0316(11) 0.0316(11) 0.0152(16) 0.000 0.000 0.0158(6) O2 0.0523(10) 0.0578(11) 0.0373(9) 0.0264(8) 0.0063(7) 0.0264(8) C10 0.0340(11) 0.0328(11) 0.0250(11) 0.0010(9) 0.0002(9) 0.0139(9) C8 0.0570(17) 0.0537(16) 0.0266(13) 0.0221(12) 0.0134(12) 0.0218(14) C2 0.0475(16) 0.0467(15) 0.0105(11) 0.0138(10) 0.0045(11) 0.0194(13) C5 0.0601(18) 0.0539(16) 0.0266(13) 0.0211(12) 0.0133(12) 0.0210(15) O1 0.0483(11) 0.0591(11) 0.0514(11) 0.0376(9) 0.0121(8) 0.0247(9) C1 0.0385(12) 0.0316(11) 0.0185(10) 0.0018(9) 0.0003(10) 0.0156(10) C11 0.0535(16) 0.0605(16) 0.0300(13) 0.0255(10) 0.0142(11) 0.0274(14) C9 0.0395(12) 0.0392(12) 0.0315(11) 0.0025(10) -0.0005(9) 0.0197(10) C13 0.0662(18) 0.118(2) 0.0590(16) 0.0600(17) 0.0315(14) 0.0624(18) C3 0.061(2) 0.131(3) 0.096(2) 0.077(2) 0.0131(17) 0.051(2) C4 0.0504(18) 0.133(3) 0.113(2) 0.094(2) 0.0191(17) 0.0452(18) C7 0.0588(19) 0.129(3) 0.100(2) 0.091(2) 0.0243(17) 0.0448(18) C12 0.0608(19) 0.104(2) 0.0720(18) 0.0564(18) 0.0194(15) 0.0502(17) C6 0.067(2) 0.134(3) 0.112(2) 0.094(2) 0.0190(17) 0.051(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 Fe1 O3 1.9138(4) . ? Fe1 O2 2.0080(14) . ? Fe1 O2 2.0081(14) 16 ? Fe1 O1 2.0100(14) 5_565 ? Fe1 O1 2.0100(14) 14_565 ? Fe1 O4 2.041(2) . ? C14 C10 1.5177(19) 11_554 ? C14 C10 1.5177(19) 7_674 ? C14 C10 1.5178(19) . ? C14 C10 1.5178(19) 4_675 ? O3 Fe1 1.9139(4) 3_665 ? O3 Fe1 1.9139(4) 14_565 ? O2 C1 1.250(2) . ? C10 C11 1.378(3) . ? C10 C9 1.387(2) . ? C8 C13 1.375(3) . ? C8 C9 1.406(3) . ? C8 C5 1.500(3) . ? C2 C7 1.355(3) . ? C2 C3 1.365(3) . ? C2 C1 1.477(3) . ? C5 C4 1.361(3) . ? C5 C6 1.388(3) . ? O1 C1 1.248(2) . ? O1 Fe1 2.0100(14) 3_665 ? C11 C12 1.384(3) . ? C11 C11 1.464(4) 7_674 ? C13 C12 1.374(3) . ? C3 C4 1.390(3) . ? C7 C6 1.386(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 O3 Fe1 O2 94.89(4) . . ? O3 Fe1 O2 94.89(5) . 16 ? O2 Fe1 O2 90.51(9) . 16 ? O3 Fe1 O1 94.59(4) . 5_565 ? O2 Fe1 O1 88.20(6) . 5_565 ? O2 Fe1 O1 170.50(6) 16 5_565 ? O3 Fe1 O1 94.59(4) . 14_565 ? O2 Fe1 O1 170.50(6) . 14_565 ? O2 Fe1 O1 88.20(6) 16 14_565 ? O1 Fe1 O1 91.52(10) 5_565 14_565 ? O3 Fe1 O4 179.75(6) . . ? O2 Fe1 O4 85.28(6) . . ? O2 Fe1 O4 85.28(6) 16 . ? O1 Fe1 O4 85.24(6) 5_565 . ? O1 Fe1 O4 85.24(6) 14_565 . ? C10 C14 C10 113.59(13) 11_554 7_674 ? C10 C14 C10 113.69(14) 11_554 . ? C10 C14 C10 101.42(15) 7_674 . ? C10 C14 C10 101.42(15) 11_554 4_675 ? C10 C14 C10 113.69(14) 7_674 4_675 ? C10 C14 C10 113.59(13) . 4_675 ? Fe1 O3 Fe1 120.002(3) 3_665 . ? Fe1 O3 Fe1 120.000(1) 3_665 14_565 ? Fe1 O3 Fe1 119.998(1) . 14_565 ? C1 O2 Fe1 134.05(13) . . ? C11 C10 C9 120.75(18) . . ? C11 C10 C14 110.54(15) . . ? C9 C10 C14 128.69(17) . . ? C13 C8 C9 119.2(2) . . ? C13 C8 C5 121.8(2) . . ? C9 C8 C5 118.9(2) . . ? C7 C2 C3 117.7(2) . . ? C7 C2 C1 121.7(2) . . ? C3 C2 C1 120.5(2) . . ? C4 C5 C6 116.7(2) . . ? C4 C5 C8 123.5(2) . . ? C6 C5 C8 119.8(2) . . ? C1 O1 Fe1 134.13(13) . 3_665 ? O1 C1 O2 123.86(19) . . ? O1 C1 C2 117.7(2) . . ? O2 C1 C2 118.4(2) . . ? C10 C11 C12 119.94(18) . . ? C10 C11 C11 108.74(11) . 7_674 ? C12 C11 C11 131.32(13) . 7_674 ? C10 C9 C8 119.04(19) . . ? C12 C13 C8 121.4(2) . . ? C2 C3 C4 121.3(2) . . ? C5 C4 C3 121.7(2) . . ? C2 C7 C6 121.5(2) . . ? C13 C12 C11 119.6(2) . . ? C7 C6 C5 121.2(2) . . ? _refine_diff_density_max 0.351 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.028 _shelx_res_file ; C:\PCN-168\250K\PCN-168-250K.res created by SHELXL-2014/7 REM reset to P6/mcc #192 REM REM REM REM p in P6/mcc #192 REM R1 = 0.1504 for 3477 Fo > 4sig(Fo) and 0.1683 for all 4208 data REM 153 parameters refined using 12 restraints REM Highest difference peak 1.444, deepest hole -0.484, 1-sigma level 0.151 REM p in P6/mcc #192 REM R1 = 0.1516 for 3477 Fo > 4sig(Fo) and 0.1688 for all 4208 data REM 153 parameters refined using 18 restraints REM Highest difference peak 1.444, deepest hole -0.473, 1-sigma level 0.150 TITL p in P6/mcc #192 CELL 1.54184 31.3244 31.3244 33.2713 90.000 90.000 120.000 ZERR 6.0000 0.0010 0.0000 0.0013 0.000 0.000 0.000 LATT 1 SYMM X-Y, X, Z SYMM -Y, X-Y, Z SYMM -X, -Y, Z SYMM -X+Y, -X, Z SYMM Y, -X+Y, Z SYMM X-Y, -Y, 0.5-Z SYMM -X, -X+Y, 0.5-Z SYMM Y, X, 0.5-Z SYMM -Y, -X, 0.5-Z SYMM -X+Y, Y, 0.5-Z SYMM X, X-Y, 0.5-Z SFAC C H O FE UNIT 318 196.0002 64.0002 12 MERG 2 FMAP 2 GRID PLAN 20 TEMP -23 ISOR 0.002 0.004 C1 C9 C10 BOND L.S. 20 ACTA WGHT 0.200000 FVAR 1.60798 FE1 4 0.401661 0.716036 0.000000 10.50000 0.03986 0.03829 = 0.00548 0.00000 0.00000 0.02187 C14 1 0.500000 1.000000 -0.250000 10.25000 0.03849 0.03180 = 0.01706 0.00000 0.00000 0.01590 O4 3 0.474621 0.768464 0.000000 10.50000 0.04374 0.05859 = 0.07224 0.00000 0.00000 0.02117 O3 3 0.333333 0.666667 0.000000 10.16667 0.03164 0.03164 = 0.01518 0.00000 0.00000 0.01582 O2 3 0.394903 0.757401 -0.042865 11.00000 0.05231 0.05783 = 0.03734 0.02636 0.00625 0.02643 C10 1 0.454017 0.969400 -0.225017 11.00000 0.03398 0.03276 = 0.02499 0.00096 0.00021 0.01394 C8 1 0.399019 0.908675 -0.177635 11.00000 0.05695 0.05367 = 0.02660 0.02206 0.01339 0.02184 C2 1 0.369483 0.798039 -0.087811 11.00000 0.04746 0.04666 = 0.01051 0.01378 0.00453 0.01939 C5 1 0.389995 0.870517 -0.146421 11.00000 0.06013 0.05392 = 0.02658 0.02114 0.01332 0.02096 O1 3 0.316497 0.736678 -0.043281 11.00000 0.04833 0.05909 = 0.05139 0.03756 0.01215 0.02471 C1 1 0.359709 0.761611 -0.055778 11.00000 0.03847 0.03161 = 0.01855 0.00183 0.00025 0.01560 C11 1 0.417982 0.980673 -0.234654 11.00000 0.05350 0.06049 = 0.03001 0.02550 0.01419 0.02743 C9 1 0.445281 0.933495 -0.196646 11.00000 0.03953 0.03922 = 0.03146 0.00254 -0.00046 0.01968 AFIX 43 H9 2 0.469924 0.925857 -0.190215 11.00000 -1.20000 AFIX 0 C13 1 0.364090 0.921450 -0.186899 11.00000 0.06616 0.11809 = 0.05901 0.05998 0.03155 0.06238 AFIX 43 H13 2 0.333614 0.905776 -0.173461 11.00000 -1.20000 AFIX 0 C3 1 0.416604 0.830054 -0.099749 11.00000 0.06072 0.13097 = 0.09600 0.07699 0.01313 0.05062 AFIX 43 H3 2 0.442795 0.827734 -0.088280 11.00000 -1.20000 AFIX 0 C4 1 0.426631 0.866023 -0.128530 11.00000 0.05037 0.13264 = 0.11322 0.09439 0.01908 0.04519 AFIX 43 H4 2 0.459538 0.887795 -0.135825 11.00000 -1.20000 AFIX 0 C7 1 0.332657 0.802320 -0.105137 11.00000 0.05884 0.12896 = 0.10044 0.09092 0.02435 0.04483 AFIX 43 H7 2 0.299906 0.780799 -0.097284 11.00000 -1.20000 AFIX 0 C12 1 0.372800 0.956660 -0.215398 11.00000 0.06076 0.10368 = 0.07200 0.05636 0.01942 0.05017 AFIX 43 H12 2 0.348204 0.964386 -0.221771 11.00000 -1.20000 AFIX 0 C6 1 0.342181 0.837708 -0.134175 11.00000 0.06725 0.13352 = 0.11230 0.09387 0.01899 0.05103 AFIX 43 H6 2 0.315778 0.839523 -0.145788 11.00000 -1.20000 AFIX 0 HKLF 4 REM p in P6/mcc #192 REM R1 = 0.0431 for 3369 Fo > 4sig(Fo) and 0.0461 for all 4208 data REM 153 parameters refined using 18 restraints END WGHT 0.0809 0.0000 REM Highest difference peak 0.351, deepest hole -0.369, 1-sigma level 0.028 Q1 1 0.4013 0.7149 -0.0295 11.00000 0.05 0.35 Q2 1 0.4991 0.7896 -0.0240 11.00000 0.05 0.29 Q3 1 0.4878 0.7976 0.0166 11.00000 0.05 0.21 Q4 1 0.3333 0.6667 -0.0199 10.33333 0.05 0.20 Q5 1 0.4906 0.8101 0.0000 10.50000 0.05 0.19 Q6 1 0.5180 1.0000 -0.2500 10.50000 0.05 0.16 Q7 1 0.4021 0.7620 -0.0674 11.00000 0.05 0.16 Q8 1 0.2860 0.6319 0.0218 11.00000 0.05 0.15 Q9 1 0.3320 0.7202 -0.0211 11.00000 0.05 0.15 Q10 1 0.3642 0.8016 -0.0649 11.00000 0.05 0.15 Q11 1 0.4605 0.7345 0.0224 11.00000 0.05 0.15 Q12 1 0.3727 0.7606 -0.0218 11.00000 0.05 0.15 Q13 1 0.3141 0.7432 -0.0229 11.00000 0.05 0.13 Q14 1 0.4480 0.9900 -0.2123 11.00000 0.05 0.13 Q15 1 0.3610 0.7637 -0.0223 11.00000 0.05 0.13 Q16 1 0.3870 0.8714 -0.1176 11.00000 0.05 0.13 Q17 1 0.3586 0.7865 -0.1151 11.00000 0.05 0.13 Q18 1 0.3424 0.6893 -0.0596 11.00000 0.05 0.13 Q19 1 0.4484 0.8780 -0.1678 11.00000 0.05 0.13 Q20 1 0.3408 0.7901 -0.1170 11.00000 0.05 0.12 ; _shelx_res_checksum 12336 _shelx_hkl_file ; ; _shelx_hkl_checksum 48736 # start Validation Reply Form _vrf_THETM01_PCN-168-250K ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The limited quality of the crystals gives rise to the weak diffraction at high angle, leading to the relatively low data completeness ; _vrf_PLAT132_PCN-168-250K ; PROBLEM: Trigonal/Hexagonal a and b Differ .............. Please Check RESPONSE: a and b are equal. ; # end Validation Reply Form ##################################################################### data_PCN-168-298K _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H32.67 Fe2 O10.67' _chemical_formula_weight 951.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 192 _space_group_name_H-M_alt 'P 6/m c c' _space_group_name_Hall '-P 6 2c' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 31.2164(8) _cell_length_b 31.216 _cell_length_c 33.3866(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 28175.3(17) _cell_formula_units_Z 6 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9857 _cell_measurement_theta_min 2.6469 _cell_measurement_theta_max 44.6962 _exptl_crystal_description Rod-like _exptl_crystal_colour Dark-red _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 0.337 _exptl_crystal_F_000 2928 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 1.364 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.3279 _exptl_absorpt_correction_T_max 0.7488 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3876 _diffrn_reflns_av_unetI/netI 0.0371 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.647 _diffrn_reflns_theta_max 44.848 _diffrn_reflns_theta_full 44.848 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 3876 _reflns_number_gt 2979 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _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. ; _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2014)' _computing_publication_material 'SHELXTL (Sheldrick, 2014)' _refine_special_details ; ? ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.003 -0.006 -0.004 23517 4338 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3876 _refine_ls_number_parameters 153 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 0.470 _refine_ls_restrained_S_all 0.475 _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_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 0.40190(2) 0.71637(2) 0.0000 0.0332(3) Uani 1 2 d S T P . . C14 C 0.5000 1.0000 -0.2500 0.0361(10) Uani 1 4 d S T P . . O4 O 0.47536(8) 0.76970(8) 0.0000 0.0726(7) Uani 1 2 d S T P . . O3 O 0.3333 0.6667 0.0000 0.0272(7) Uani 1 6 d S T P . . O1 O 0.39547(6) 0.75776(6) -0.04238(4) 0.0579(5) Uani 1 1 d . . . . . C10 C 0.45404(8) 0.96966(8) -0.22512(5) 0.0395(6) Uani 1 1 d . U . . . C5 C 0.38949(10) 0.87019(9) -0.14663(6) 0.0584(7) Uani 1 1 d . . . . . C8 C 0.39928(10) 0.90825(9) -0.17771(6) 0.0587(7) Uani 1 1 d . . . . . C2 C 0.36939(9) 0.79824(8) -0.08775(6) 0.0455(6) Uani 1 1 d . U . . . C9 C 0.44531(8) 0.93355(8) -0.19680(6) 0.0455(6) Uani 1 1 d . U . . . H9 H 0.4700 0.9262 -0.1906 0.055 Uiso 1 1 calc R U . . . O2 O 0.31636(6) 0.73692(6) -0.04317(5) 0.0611(5) Uani 1 1 d . . . . . C1 C 0.36024(10) 0.76159(8) -0.05558(6) 0.0366(6) Uani 1 1 d . U . . . C11 C 0.41793(10) 0.98052(9) -0.23518(6) 0.0604(7) Uani 1 1 d . . . . . C3 C 0.41646(12) 0.83100(12) -0.09900(8) 0.1086(11) Uani 1 1 d . . . . . H3 H 0.4425 0.8293 -0.0872 0.130 Uiso 1 1 calc R U . . . C13 C 0.36348(11) 0.92069(11) -0.18706(7) 0.0974(10) Uani 1 1 d . . . . . H13 H 0.3331 0.9047 -0.1740 0.117 Uiso 1 1 calc R U . . . C6 C 0.34166(11) 0.83721(12) -0.13470(8) 0.1099(12) Uani 1 1 d . . . . . H6 H 0.3154 0.8388 -0.1463 0.132 Uiso 1 1 calc R U . . . C7 C 0.33236(10) 0.80199(11) -0.10590(8) 0.1006(11) Uani 1 1 d . . . . . H7 H 0.2998 0.7801 -0.0986 0.121 Uiso 1 1 calc R U . . . C4 C 0.42653(10) 0.86686(11) -0.12768(9) 0.1046(11) Uani 1 1 d . . . . . H4 H 0.4593 0.8892 -0.1342 0.126 Uiso 1 1 calc R U . . . C12 C 0.37231(11) 0.95673(11) -0.21571(8) 0.0963(10) Uani 1 1 d . . . . . H12 H 0.3481 0.9648 -0.2217 0.116 Uiso 1 1 calc R U . . . 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 0.0490(4) 0.0463(4) 0.0066(3) 0.000 0.000 0.0255(3) C14 0.047(2) 0.039(3) 0.019(2) 0.000 0.000 0.0197(13) O4 0.0557(15) 0.0758(16) 0.0754(15) 0.000 0.000 0.0247(13) O3 0.0339(12) 0.0339(12) 0.0137(16) 0.000 0.000 0.0170(6) O1 0.0577(11) 0.0712(12) 0.0443(10) 0.0309(8) 0.0027(8) 0.0319(9) C10 0.0479(14) 0.0464(14) 0.0207(13) 0.0042(12) -0.0017(10) 0.0209(12) C5 0.076(2) 0.0692(19) 0.0251(13) 0.0281(13) 0.0164(14) 0.0331(17) C8 0.0676(19) 0.0732(18) 0.0325(14) 0.0233(14) 0.0104(14) 0.0331(16) C2 0.0488(16) 0.0517(15) 0.0275(13) 0.0105(12) 0.0017(13) 0.0188(14) C9 0.0543(17) 0.0540(15) 0.0271(12) 0.0059(12) -0.0011(11) 0.0263(13) O2 0.0631(12) 0.0678(11) 0.0519(11) 0.0373(9) 0.0122(9) 0.0325(10) C1 0.0546(17) 0.0373(14) 0.0070(12) 0.0041(11) 0.0047(12) 0.0148(14) C11 0.0660(17) 0.0811(19) 0.0331(14) 0.0371(12) 0.0199(13) 0.0361(16) C3 0.077(3) 0.153(3) 0.091(2) 0.088(2) 0.0098(18) 0.054(2) C13 0.091(2) 0.153(3) 0.0703(18) 0.080(2) 0.0454(17) 0.078(2) C6 0.075(2) 0.145(3) 0.107(2) 0.102(2) 0.0243(18) 0.053(2) C7 0.061(2) 0.134(3) 0.095(2) 0.086(2) 0.0209(17) 0.0401(18) C4 0.064(2) 0.146(3) 0.106(2) 0.093(2) 0.0251(18) 0.055(2) C12 0.090(2) 0.136(3) 0.0792(19) 0.074(2) 0.0261(18) 0.069(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 Fe1 O3 1.9150(4) . ? Fe1 O1 1.9925(15) 16 ? Fe1 O1 1.9927(15) . ? Fe1 O2 2.0138(16) 5_565 ? Fe1 O2 2.0138(16) 14_565 ? Fe1 O4 2.053(2) . ? C14 C10 1.512(2) 4_675 ? C14 C10 1.512(2) 11_554 ? C14 C10 1.512(2) 7_674 ? C14 C10 1.512(2) . ? O3 Fe1 1.9150(4) 3_665 ? O3 Fe1 1.9150(4) 14_565 ? O1 C1 1.245(2) . ? C10 C11 1.371(3) . ? C10 C9 1.390(3) . ? C5 C4 1.367(3) . ? C5 C6 1.382(3) . ? C5 C8 1.490(3) . ? C8 C13 1.389(3) . ? C8 C9 1.400(3) . ? C2 C7 1.361(3) . ? C2 C3 1.358(3) . ? C2 C1 1.489(3) . ? O2 C1 1.260(2) . ? O2 Fe1 2.0138(16) 3_665 ? C11 C12 1.394(3) . ? C11 C11 1.445(4) 7_674 ? C3 C4 1.385(3) . ? C13 C12 1.395(3) . ? C6 C7 1.378(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 O3 Fe1 O1 95.24(5) . 16 ? O3 Fe1 O1 95.23(5) . . ? O1 Fe1 O1 90.47(9) 16 . ? O3 Fe1 O2 94.51(5) . 5_565 ? O1 Fe1 O2 170.25(6) 16 5_565 ? O1 Fe1 O2 88.24(7) . 5_565 ? O3 Fe1 O2 94.51(5) . 14_565 ? O1 Fe1 O2 88.24(7) 16 14_565 ? O1 Fe1 O2 170.25(6) . 14_565 ? O2 Fe1 O2 91.40(10) 5_565 14_565 ? O3 Fe1 O4 179.94(7) . . ? O1 Fe1 O4 84.72(7) 16 . ? O1 Fe1 O4 84.72(7) . . ? O2 Fe1 O4 85.54(7) 5_565 . ? O2 Fe1 O4 85.54(7) 14_565 . ? C10 C14 C10 101.06(17) 4_675 11_554 ? C10 C14 C10 114.31(15) 4_675 7_674 ? C10 C14 C10 113.35(14) 11_554 7_674 ? C10 C14 C10 113.35(14) 4_675 . ? C10 C14 C10 114.31(15) 11_554 . ? C10 C14 C10 101.06(17) 7_674 . ? Fe1 O3 Fe1 120.002(2) 3_665 . ? Fe1 O3 Fe1 120.000(1) 3_665 14_565 ? Fe1 O3 Fe1 119.998(1) . 14_565 ? C1 O1 Fe1 133.95(14) . . ? C11 C10 C9 121.00(19) . . ? C11 C10 C14 110.51(17) . . ? C9 C10 C14 128.43(19) . . ? C4 C5 C6 116.7(2) . . ? C4 C5 C8 122.6(2) . . ? C6 C5 C8 120.6(2) . . ? C13 C8 C9 118.8(2) . . ? C13 C8 C5 120.4(2) . . ? C9 C8 C5 120.7(2) . . ? C7 C2 C3 117.3(2) . . ? C7 C2 C1 122.9(2) . . ? C3 C2 C1 119.8(2) . . ? C10 C9 C8 119.8(2) . . ? C1 O2 Fe1 133.32(14) . 3_665 ? O1 C1 O2 124.58(19) . . ? O1 C1 C2 119.4(2) . . ? O2 C1 C2 116.0(2) . . ? C10 C11 C12 120.1(2) . . ? C10 C11 C11 108.90(13) . 7_674 ? C12 C11 C11 130.95(14) . 7_674 ? C2 C3 C4 121.5(2) . . ? C8 C13 C12 121.1(2) . . ? C7 C6 C5 120.9(2) . . ? C2 C7 C6 122.0(2) . . ? C5 C4 C3 121.5(2) . . ? C13 C12 C11 119.1(2) . . ? _refine_diff_density_max 0.295 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.026 _shelx_res_file ; C:\PCN-168\298K\PCN-168-298K.res created by SHELXL-2014/7 REM reset to P6/mcc #192 REM REM REM REM p in P6/mcc #192 REM R1 = 0.1538 for 3125 Fo > 4sig(Fo) and 0.1747 for all 3876 data REM 153 parameters refined using 0 restraints REM Highest difference peak 1.199, deepest hole -0.513, 1-sigma level 0.147 REM p in P6/mcc #192 REM R1 = 0.1518 for 3125 Fo > 4sig(Fo) and 0.1722 for all 3876 data REM 153 parameters refined using 24 restraints REM Highest difference peak 1.207, deepest hole -0.487, 1-sigma level 0.151 TITL p in P6/mcc #192 CELL 1.54184 31.2164 31.2164 33.3866 90.000 90.000 120.000 ZERR 6.0000 0.0008 0.0000 0.0011 0.000 0.000 0.000 LATT 1 SYMM X-Y, X, Z SYMM -Y, X-Y, Z SYMM -X, -Y, Z SYMM -X+Y, -X, Z SYMM Y, -X+Y, Z SYMM X-Y, -Y, 0.5-Z SYMM -X, -X+Y, 0.5-Z SYMM Y, X, 0.5-Z SYMM -Y, -X, 0.5-Z SYMM -X+Y, Y, 0.5-Z SYMM X, X-Y, 0.5-Z SFAC C H O FE UNIT 318 196.0002 64.0002 12 MERG 2 FMAP 2 GRID PLAN 20 TEMP 25 BOND ISOR 0.005 C1 C2 C9 C10 L.S. 20 ACTA WGHT 0.200000 FVAR 1.72986 FE1 4 0.401896 0.716367 0.000000 10.50000 0.04899 0.04626 = 0.00660 0.00000 0.00000 0.02550 C14 1 0.500000 1.000000 -0.250000 10.25000 0.04707 0.03934 = 0.01937 0.00000 0.00000 0.01967 O4 3 0.475364 0.769696 0.000000 10.50000 0.05568 0.07577 = 0.07538 0.00000 0.00000 0.02473 O3 3 0.333333 0.666667 0.000000 10.16667 0.03393 0.03393 = 0.01372 0.00000 0.00000 0.01697 O1 3 0.395467 0.757759 -0.042376 11.00000 0.05768 0.07118 = 0.04430 0.03086 0.00269 0.03190 C10 1 0.454039 0.969662 -0.225117 11.00000 0.04789 0.04638 = 0.02072 0.00423 -0.00167 0.02094 C5 1 0.389487 0.870187 -0.146629 11.00000 0.07647 0.06917 = 0.02511 0.02809 0.01637 0.03310 C8 1 0.399276 0.908252 -0.177709 11.00000 0.06764 0.07319 = 0.03247 0.02326 0.01039 0.03306 C2 1 0.369386 0.798242 -0.087749 11.00000 0.04885 0.05173 = 0.02751 0.01048 0.00175 0.01883 C9 1 0.445305 0.933553 -0.196804 11.00000 0.05428 0.05403 = 0.02710 0.00591 -0.00108 0.02625 AFIX 43 H9 2 0.469966 0.926216 -0.190559 11.00000 -1.20000 AFIX 0 O2 3 0.316363 0.736916 -0.043168 11.00000 0.06307 0.06783 = 0.05192 0.03731 0.01215 0.03248 C1 1 0.360245 0.761587 -0.055584 11.00000 0.05457 0.03733 = 0.00698 0.00411 0.00469 0.01477 C11 1 0.417926 0.980521 -0.235183 11.00000 0.06595 0.08113 = 0.03314 0.03712 0.01991 0.03613 C3 1 0.416460 0.831001 -0.098996 11.00000 0.07728 0.15263 = 0.09081 0.08766 0.00984 0.05358 AFIX 43 H3 2 0.442545 0.829316 -0.087157 11.00000 -1.20000 AFIX 0 C13 1 0.363482 0.920689 -0.187059 11.00000 0.09098 0.15323 = 0.07034 0.08010 0.04540 0.07771 AFIX 43 H13 2 0.333113 0.904713 -0.173995 11.00000 -1.20000 AFIX 0 C6 1 0.341662 0.837211 -0.134699 11.00000 0.07463 0.14479 = 0.10725 0.10181 0.02434 0.05263 AFIX 43 H6 2 0.315400 0.838815 -0.146271 11.00000 -1.20000 AFIX 0 C7 1 0.332364 0.801995 -0.105896 11.00000 0.06086 0.13403 = 0.09538 0.08643 0.02089 0.04014 AFIX 43 H7 2 0.299786 0.780116 -0.098635 11.00000 -1.20000 AFIX 0 C4 1 0.426534 0.866860 -0.127682 11.00000 0.06433 0.14629 = 0.10599 0.09344 0.02511 0.05478 AFIX 43 H4 2 0.459259 0.889195 -0.134209 11.00000 -1.20000 AFIX 0 C12 1 0.372315 0.956732 -0.215708 11.00000 0.08993 0.13608 = 0.07919 0.07428 0.02608 0.06875 AFIX 43 H12 2 0.348102 0.964783 -0.221735 11.00000 -1.20000 AFIX 0 HKLF 4 REM p in P6/mcc #192 REM R1 = 0.0401 for 2979 Fo > 4sig(Fo) and 0.0438 for all 3876 data REM 153 parameters refined using 24 restraints END WGHT 0.0737 0.0000 REM Highest difference peak 0.295, deepest hole -0.331, 1-sigma level 0.026 Q1 1 0.3999 0.7119 -0.0293 11.00000 0.05 0.30 Q2 1 0.5008 0.7913 -0.0239 11.00000 0.05 0.28 Q3 1 0.3392 0.7128 -0.0216 11.00000 0.05 0.22 Q4 1 0.4510 0.7398 -0.0217 11.00000 0.05 0.18 Q5 1 0.3847 0.8723 -0.1161 11.00000 0.05 0.17 Q6 1 0.3672 0.7623 -0.0214 11.00000 0.05 0.16 Q7 1 0.4718 0.7578 0.0140 11.00000 0.05 0.15 Q8 1 0.4105 0.7595 -0.0691 11.00000 0.05 0.13 Q9 1 0.4294 0.8321 -0.0679 11.00000 0.05 0.13 Q10 1 0.5158 1.0000 -0.2500 10.50000 0.05 0.13 Q11 1 0.3598 0.7912 -0.1193 11.00000 0.05 0.12 Q12 1 0.3826 0.8099 -0.0671 11.00000 0.05 0.12 Q13 1 0.3338 0.7266 -0.0640 11.00000 0.05 0.11 Q14 1 0.4383 0.9865 -0.2061 11.00000 0.05 0.11 Q15 1 0.3333 0.6667 0.0537 10.33333 0.05 0.10 Q16 1 0.3689 0.7605 -0.0891 11.00000 0.05 0.10 Q17 1 0.3492 0.8271 -0.0871 11.00000 0.05 0.10 Q18 1 0.2675 0.7219 -0.0631 11.00000 0.05 0.09 Q19 1 0.4608 0.8086 -0.0450 11.00000 0.05 0.09 Q20 1 0.3441 0.8028 -0.0838 11.00000 0.05 0.09 ; _shelx_res_checksum 75283 _shelx_hkl_file ; ; _shelx_hkl_checksum 49930 # start Validation Reply Form _vrf_THETM01_PCN-168-298K ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The limited quality of the crystals gives rise to the weak diffraction at high angle, leading to the relatively low data completeness ; _vrf_PLAT132_PCN-168-298K ; PROBLEM: Trigonal/Hexagonal a and b Differ .............. Please Check RESPONSE: a and b are equal. ; # end Validation Reply Form ##################################################################### data_PCN-168-150K-down _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H32.67 Fe2 O10.67' _chemical_formula_weight 951.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 192 _space_group_name_H-M_alt 'P 6/m c c' _space_group_name_Hall '-P 6 2c' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 29.2327(15) _cell_length_b 29.233 _cell_length_c 35.385(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 26187(3) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6017 _cell_measurement_theta_min 2.4974 _cell_measurement_theta_max 36.9155 _exptl_crystal_description Rod-like _exptl_crystal_colour Dark-red _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 0.362 _exptl_crystal_F_000 2928 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 1.467 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.3170 _exptl_absorpt_correction_T_max 0.7473 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 2236 _diffrn_reflns_av_unetI/netI 0.0710 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_limit_h_min 20 _diffrn_reflns_limit_h_max -20 _diffrn_reflns_limit_k_min 22 _diffrn_reflns_limit_k_max -21 _diffrn_reflns_limit_l_min 27 _diffrn_reflns_limit_l_max -26 _diffrn_reflns_theta_min 2.497 _diffrn_reflns_theta_max 36.923 _diffrn_reflns_theta_full 36.923 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 2236 _reflns_number_gt 1536 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _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. ; _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'S'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2014)' _computing_publication_material 'SHELXTL (Sheldrick, 2014)' _refine_special_details ; ? ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.004 -0.006 -0.003 21730 5920 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0789P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2236 _refine_ls_number_parameters 153 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.933 _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_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 0.72042(4) 0.31451(4) 0.0000 0.0449(6) Uani 1 2 d S T P . . O1 O 0.73992(19) 0.42697(17) 0.04179(12) 0.0808(19) Uani 1 1 d . . . . . O4 O 0.77703(18) 0.29470(17) 0.0000 0.0728(17) Uani 1 2 d S T P . . O2 O 0.76338(19) 0.36552(18) 0.04131(12) 0.0795(19) Uani 1 1 d . . . . . C5 C 0.8705(3) 0.4835(5) 0.1465(3) 0.061(2) Uani 1 1 d . . . . . C2 C 0.7994(3) 0.4336(4) 0.0852(3) 0.073(3) Uani 1 1 d . U . . . C11 C 0.9790(2) 0.5643(4) 0.23448(16) 0.063(2) Uani 1 1 d . . . . . C14 C 1.0000 0.5000 0.2500 0.046(4) Uani 1 4 d S T P . . C10 C 0.9688(3) 0.5164(4) 0.22682(19) 0.053(2) Uani 1 1 d . U . . . O3 O 0.6667 0.3333 0.0000 0.045(2) Uani 1 6 d S T P . . C8 C 0.9069(3) 0.5128(4) 0.1791(2) 0.057(2) Uani 1 1 d . . . . . C9 C 0.9323(3) 0.4893(2) 0.19812(18) 0.0440(18) Uani 1 1 d . U . . . H9 H 0.9246 0.4548 0.1913 0.053 Uiso 1 1 calc R U . . . C4 C 0.8660(4) 0.4410(6) 0.1322(4) 0.137(4) Uani 1 1 d . . . . . H4 H 0.8874 0.4272 0.1411 0.165 Uiso 1 1 calc R U . . . C13 C 0.9185(3) 0.5625(5) 0.1872(2) 0.069(2) Uani 1 1 d . . . . . H13 H 0.9025 0.5785 0.1732 0.083 Uiso 1 1 calc R U . . . C3 C 0.8282(5) 0.4146(3) 0.1027(4) 0.143(4) Uani 1 1 d . . . . . H3 H 0.8228 0.3812 0.0946 0.171 Uiso 1 1 calc R U . . . C12 C 0.9545(4) 0.5908(3) 0.2164(3) 0.093(3) Uani 1 1 d . . . . . H12 H 0.9621 0.6252 0.2236 0.112 Uiso 1 1 calc R U . . . C1 C 0.7620(3) 0.4033(3) 0.0505(2) 0.052(3) Uani 1 1 d . . . . . C6 C 0.8420(5) 0.5027(3) 0.1328(3) 0.132(3) Uani 1 1 d . . . . . H6 H 0.8453 0.5344 0.1427 0.158 Uiso 1 1 calc R U . . . C7 C 0.8038(4) 0.4736(6) 0.1012(3) 0.128(3) Uani 1 1 d . . . . . H7 H 0.7816 0.4866 0.0929 0.154 Uiso 1 1 calc R U . . . 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 0.0512(10) 0.0507(10) 0.0283(8) 0.000 0.000 0.0222(9) O1 0.117(5) 0.068(4) 0.079(3) -0.015(3) -0.006(3) 0.062(3) O4 0.083(4) 0.073(4) 0.062(3) 0.000 0.000 0.039(4) O2 0.107(4) 0.103(5) 0.062(3) -0.003(3) -0.009(3) 0.077(4) C5 0.075(7) 0.056(9) 0.061(7) -0.007(7) -0.020(6) 0.038(7) C2 0.080(5) 0.071(5) 0.080(5) 0.002(4) 0.004(4) 0.048(4) C11 0.067(6) 0.079(7) 0.060(6) 0.020(5) -0.001(4) 0.049(6) C14 0.034(10) 0.055(9) 0.043(10) 0.000 0.000 0.017(5) C10 0.058(4) 0.042(4) 0.052(4) -0.007(4) -0.004(3) 0.020(4) O3 0.053(4) 0.053(4) 0.029(5) 0.000 0.000 0.026(2) C8 0.068(6) 0.055(8) 0.062(7) -0.006(7) 0.000(5) 0.041(6) C9 0.052(4) 0.036(4) 0.049(4) -0.004(3) 0.007(3) 0.026(3) C4 0.160(11) 0.119(10) 0.148(10) -0.040(8) -0.053(8) 0.082(9) C13 0.085(7) 0.082(8) 0.059(6) 0.005(6) -0.013(5) 0.056(6) C3 0.163(9) 0.095(8) 0.153(9) -0.053(7) -0.026(7) 0.052(8) C12 0.106(7) 0.074(7) 0.082(7) -0.030(6) 0.000(5) 0.031(6) C1 0.069(7) 0.050(8) 0.048(6) 0.000(6) 0.015(5) 0.038(6) C6 0.173(10) 0.115(8) 0.124(9) -0.040(8) -0.038(7) 0.084(9) C7 0.142(9) 0.149(10) 0.112(8) -0.010(6) -0.039(7) 0.087(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O3 1.9070(12) . ? Fe1 O4 2.008(5) . ? Fe1 O2 2.016(5) . ? Fe1 O2 2.016(5) 16 ? Fe1 O1 2.029(5) 14_665 ? Fe1 O1 2.029(5) 5_665 ? O1 C1 1.199(6) . ? O1 Fe1 2.029(5) 3_655 ? O2 C1 1.171(6) . ? C5 C4 1.289(9) . ? C5 C6 1.307(10) . ? C5 C8 1.509(10) . ? C2 C7 1.246(9) . ? C2 C3 1.368(11) . ? C2 C1 1.587(11) . ? C11 C10 1.307(7) . ? C11 C12 1.442(7) . ? C11 C11 1.530(13) 8_765 ? C14 C10 1.473(6) 8_765 ? C14 C10 1.473(6) 12 ? C14 C10 1.473(6) 4_765 ? C14 C10 1.473(6) . ? C10 C9 1.396(7) . ? O3 Fe1 1.9070(12) 14_665 ? O3 Fe1 1.9069(11) 3_655 ? C8 C13 1.347(7) . ? C8 C9 1.411(7) . ? C4 C3 1.434(10) . ? C13 C12 1.409(7) . ? C6 C7 1.508(9) . ? 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 O3 Fe1 O4 179.99(14) . . ? O3 Fe1 O2 94.87(13) . . ? O4 Fe1 O2 85.12(16) . . ? O3 Fe1 O2 94.88(13) . 16 ? O4 Fe1 O2 85.12(16) . 16 ? O2 Fe1 O2 92.9(2) . 16 ? O3 Fe1 O1 94.81(12) . 14_665 ? O4 Fe1 O1 85.20(16) . 14_665 ? O2 Fe1 O1 170.31(16) . 14_665 ? O2 Fe1 O1 85.92(15) 16 14_665 ? O3 Fe1 O1 94.81(12) . 5_665 ? O4 Fe1 O1 85.20(16) . 5_665 ? O2 Fe1 O1 85.93(15) . 5_665 ? O2 Fe1 O1 170.31(16) 16 5_665 ? O1 Fe1 O1 93.6(2) 14_665 5_665 ? C1 O1 Fe1 125.4(6) . 3_655 ? C1 O2 Fe1 126.6(6) . . ? C4 C5 C6 119.3(10) . . ? C4 C5 C8 123.4(12) . . ? C6 C5 C8 117.3(12) . . ? C7 C2 C3 112.3(10) . . ? C7 C2 C1 126.5(11) . . ? C3 C2 C1 121.0(12) . . ? C10 C11 C12 125.2(8) . . ? C10 C11 C11 106.6(5) . 8_765 ? C12 C11 C11 128.2(6) . 8_765 ? C10 C14 C10 112.3(6) 8_765 12 ? C10 C14 C10 115.1(5) 8_765 4_765 ? C10 C14 C10 101.2(8) 12 4_765 ? C10 C14 C10 101.2(8) 8_765 . ? C10 C14 C10 115.1(5) 12 . ? C10 C14 C10 112.3(6) 4_765 . ? C11 C10 C9 117.2(6) . . ? C11 C10 C14 112.8(9) . . ? C9 C10 C14 130.0(9) . . ? Fe1 O3 Fe1 119.997(3) . 14_665 ? Fe1 O3 Fe1 119.996(1) . 3_655 ? Fe1 O3 Fe1 120.006(2) 14_665 3_655 ? C13 C8 C9 120.8(8) . . ? C13 C8 C5 120.0(8) . . ? C9 C8 C5 118.9(9) . . ? C10 C9 C8 120.8(6) . . ? C5 C4 C3 119.0(10) . . ? C8 C13 C12 120.1(9) . . ? C2 C3 C4 125.2(10) . . ? C13 C12 C11 115.8(7) . . ? O2 C1 O1 139.0(10) . . ? O2 C1 C2 113.7(9) . . ? O1 C1 C2 107.3(8) . . ? C5 C6 C7 118.9(9) . . ? C2 C7 C6 124.6(10) . . ? _refine_diff_density_max 0.237 _refine_diff_density_min -0.176 _refine_diff_density_rms 0.027 _shelx_res_file ; C:\PCN-168\150K-down\PCN-168-150K-down.res created by SHELXL-2014/7 REM reset to P6/mcc #192 REM REM REM REM p in P6/mcc #192 REM R1 = 0.2754 for 1693 Fo > 4sig(Fo) and 0.3061 for all 2236 data REM 69 parameters refined using 0 restraints REM Highest difference peak 1.470, deepest hole -0.840, 1-sigma level 0.203 REM p in P6/mcc #192 REM R1 = 0.2726 for 1693 Fo > 4sig(Fo) and 0.3031 for all 2236 data REM 69 parameters refined using 0 restraints REM Highest difference peak 1.494, deepest hole -0.815, 1-sigma level 0.198 TITL p in P6/mcc #192 CELL 1.54184 29.2327 29.2327 35.3847 90.000 90.000 120.000 ZERR 6.0000 0.0015 0.0000 0.0020 0.000 0.000 0.000 LATT 1 SYMM X-Y, X, Z SYMM -Y, X-Y, Z SYMM -X, -Y, Z SYMM -X+Y, -X, Z SYMM Y, -X+Y, Z SYMM X-Y, -Y, 0.5-Z SYMM -X, -X+Y, 0.5-Z SYMM Y, X, 0.5-Z SYMM -Y, -X, 0.5-Z SYMM -X+Y, Y, 0.5-Z SYMM X, X-Y, 0.5-Z SFAC C H O FE UNIT 318 196.0002 64.0002 12 MERG 2 FMAP 2 GRID PLAN 20 TEMP -123 BOND ISOR 0.005 C2 C9 C10 L.S. 20 ACTA WGHT 0.078900 FVAR 1.63969 FE1 4 0.720419 0.314507 0.000000 10.50000 0.05123 0.05072 = 0.02829 0.00000 0.00000 0.02224 O1 3 0.739916 0.426972 0.041790 11.00000 0.11674 0.06844 = 0.07858 -0.01453 -0.00622 0.06238 O4 3 0.777028 0.294700 0.000000 10.50000 0.08337 0.07275 = 0.06188 0.00000 0.00000 0.03873 O2 3 0.763380 0.365518 0.041312 11.00000 0.10693 0.10255 = 0.06226 -0.00323 -0.00915 0.07739 C5 1 0.870511 0.483549 0.146526 11.00000 0.07492 0.05591 = 0.06087 -0.00745 -0.01956 0.03825 C2 1 0.799413 0.433584 0.085186 11.00000 0.08013 0.07104 = 0.07988 0.00238 0.00383 0.04796 C11 1 0.978970 0.564304 0.234482 11.00000 0.06691 0.07891 = 0.05995 0.01992 -0.00135 0.04893 C14 1 1.000000 0.500000 0.250000 10.25000 0.03374 0.05462 = 0.04323 0.00000 0.00000 0.01687 C10 1 0.968798 0.516369 0.226823 11.00000 0.05826 0.04161 = 0.05167 -0.00694 -0.00357 0.01954 O3 3 0.666667 0.333333 0.000000 10.16667 0.05277 0.05277 = 0.02891 0.00000 0.00000 0.02638 C8 1 0.906862 0.512804 0.179052 11.00000 0.06786 0.05466 = 0.06234 -0.00622 -0.00043 0.04089 C9 1 0.932341 0.489350 0.198116 11.00000 0.05181 0.03620 = 0.04936 -0.00373 0.00664 0.02601 AFIX 43 H9 2 0.924599 0.454756 0.191340 11.00000 -1.20000 AFIX 0 C4 1 0.866020 0.440955 0.132212 11.00000 0.15972 0.11942 = 0.14840 -0.04029 -0.05305 0.08189 AFIX 43 H4 2 0.887438 0.427246 0.141103 11.00000 -1.20000 AFIX 0 C13 1 0.918539 0.562516 0.187160 11.00000 0.08527 0.08161 = 0.05881 0.00488 -0.01341 0.05609 AFIX 43 H13 2 0.902528 0.578530 0.173167 11.00000 -1.20000 AFIX 0 C3 1 0.828232 0.414550 0.102673 11.00000 0.16287 0.09527 = 0.15304 -0.05313 -0.02622 0.05206 AFIX 43 H3 2 0.822778 0.381189 0.094606 11.00000 -1.20000 AFIX 0 C12 1 0.954459 0.590810 0.216359 11.00000 0.10611 0.07414 = 0.08192 -0.03011 -0.00013 0.03144 AFIX 43 H12 2 0.962054 0.625185 0.223649 11.00000 -1.20000 AFIX 0 C1 1 0.761989 0.403285 0.050511 11.00000 0.06862 0.04967 = 0.04820 -0.00023 0.01506 0.03840 C6 1 0.841996 0.502697 0.132841 11.00000 0.17275 0.11479 = 0.12440 -0.04039 -0.03839 0.08437 AFIX 43 H6 2 0.845262 0.534436 0.142676 11.00000 -1.20000 AFIX 0 C7 1 0.803847 0.473582 0.101195 11.00000 0.14248 0.14901 = 0.11200 -0.00983 -0.03922 0.08652 AFIX 43 H7 2 0.781624 0.486641 0.092872 11.00000 -1.20000 AFIX 0 HKLF 4 REM p in P6/mcc #192 REM R1 = 0.0535 for 1536 Fo > 4sig(Fo) and 0.0672 for all 2236 data REM 153 parameters refined using 18 restraints END WGHT 0.0788 0.0000 REM Highest difference peak 0.237, deepest hole -0.176, 1-sigma level 0.027 Q1 1 0.6880 0.4062 0.0413 11.00000 0.05 0.24 Q2 1 0.7561 0.2991 0.0000 10.50000 0.05 0.19 Q3 1 0.6547 0.3024 0.0000 10.50000 0.05 0.19 Q4 1 0.7011 0.2631 0.0000 10.50000 0.05 0.18 Q5 1 0.8208 0.3188 0.0000 10.50000 0.05 0.17 Q6 1 0.7416 0.3470 0.0000 10.50000 0.05 0.16 Q7 1 0.7946 0.3318 0.0334 11.00000 0.05 0.13 Q8 1 0.6606 0.3402 0.0381 11.00000 0.05 0.12 Q9 1 0.7519 0.4198 0.0879 11.00000 0.05 0.12 Q10 1 0.7522 0.4621 0.0414 11.00000 0.05 0.11 Q11 1 0.7910 0.2966 -0.0344 11.00000 0.05 0.11 Q12 1 0.7854 0.3707 0.0407 11.00000 0.05 0.10 Q13 1 0.7952 0.4206 0.0469 11.00000 0.05 0.10 Q14 1 0.7506 0.2376 0.0000 10.50000 0.05 0.10 Q15 1 0.8007 0.3557 0.0409 11.00000 0.05 0.10 Q16 1 1.0000 0.5000 0.2004 10.50000 0.05 0.09 Q17 1 0.9759 0.4520 0.2301 11.00000 0.05 0.09 Q18 1 0.8676 0.4476 0.0000 10.50000 0.05 0.08 Q19 1 0.7989 0.4625 0.0000 10.50000 0.05 0.08 Q20 1 0.9797 0.4729 0.2242 11.00000 0.05 0.07 ; _shelx_res_checksum 43361 _shelx_hkl_file ; ; _shelx_hkl_checksum 33964 # start Validation Reply Form _vrf_PLAT132_PCN-168-150K-down ; PROBLEM: Trigonal/Hexagonal a and b Differ .............. Please Check RESPONSE: a and b are equal. ; # end Validation Reply Form