#####################################################################
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