# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
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data_20161218e
_database_code_depnum_ccdc_archive 'CCDC 1547628'
_audit_update_record
;
2017-07-20 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_audit_creation_date 2017-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common ?
_chemical_name_systematic 135TIPB-FA
_chemical_formula_moiety 'C6 F3 I3, 2(C16 H10)'
_chemical_formula_sum 'C38 H20 F3 I3'
_chemical_formula_weight 914.24
_chemical_melting_point ?
_chemical_oxdiff_formula c1h1f1i1
_chemical_oxdiff_usercomment Eu
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 62
_space_group_name_H-M_alt 'P n m a'
_space_group_name_Hall '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
_cell_length_a 17.2928(9)
_cell_length_b 23.1876(10)
_cell_length_c 7.7431(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3104.8(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 6575
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 28.9190
_cell_measurement_theta_min 3.9390
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 3.065
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.80635
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour green
_exptl_crystal_colour_primary green
_exptl_crystal_density_diffrn 1.956
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description cube
_exptl_crystal_F_000 1736
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.35
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0418
_diffrn_reflns_av_unetI/netI 0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_k_min -32
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 18806
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 29.937
_diffrn_reflns_theta_min 3.376
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w 8.00 87.00 1.00 2.00 -- 12.76 37.00 0.00 79
2 \w -20.00 27.00 1.00 2.00 -- 12.76 -99.00 90.00 47
3 \w 56.00 82.00 1.00 2.00 -- 12.76-178.00 60.00 26
4 \w -59.00 -33.00 1.00 2.00 -- 12.76 -19.00-180.00 26
5 \w 35.00 100.00 1.00 2.00 -- 12.76-178.00 -60.00 65
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0278942000
_diffrn_orient_matrix_UB_12 0.0223659000
_diffrn_orient_matrix_UB_13 0.0058014000
_diffrn_orient_matrix_UB_21 0.0266469000
_diffrn_orient_matrix_UB_22 -0.0195680000
_diffrn_orient_matrix_UB_23 0.0376861000
_diffrn_orient_matrix_UB_31 0.0139569000
_diffrn_orient_matrix_UB_32 -0.0073143000
_diffrn_orient_matrix_UB_33 -0.0832520000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3428
_reflns_number_total 4188
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.986
_refine_diff_density_min -2.422
_refine_diff_density_rms 0.139
_refine_ls_extinction_coef 0.00308(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 257
_refine_ls_number_reflns 4188
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0568
_refine_ls_R_factor_gt 0.0430
_refine_ls_restrained_S_all 1.038
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+14.4871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0852
_refine_ls_wR_factor_ref 0.0929
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
Fixed Sof: C14(0.5) C15(0.5) H15(0.5) C16(0.5) H16(0.5) C17(0.5) H17(0.5)
C18(0.5) H18(0.5) C19(0.5) C20(0.5) C21(0.5) H21(0.5) C22(0.5) H22(0.5)
C23(0.5) H23(0.5) C24(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5) C27(0.5)
H27(0.5) C28(0.5) C29(0.5)
4.a Aromatic/amide H refined with riding coordinates:
C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17),
C18(H18), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27)
4.b Fitted hexagon refined as free rotating group:
C14(C15,C16,C17,C18,C19), C24(C25,C26,C27,C28,C29)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
C1 C 0.6842(3) 0.7500 0.0496(7) 0.0217(11) Uani 1 2 d S T P . .
C2 C 0.6472(2) 0.69923(16) 0.0898(5) 0.0212(8) Uani 1 1 d . . . . .
C3 C 0.5755(2) 0.69788(15) 0.1693(5) 0.0212(8) Uani 1 1 d . . . . .
C4 C 0.5412(3) 0.7500 0.2083(7) 0.0202(11) Uani 1 2 d S T P . .
C5 C 0.6875(3) 0.64732(19) 0.5340(6) 0.0313(10) Uani 1 1 d . . . . .
H5 H 0.6625 0.6134 0.5650 0.038 Uiso 1 1 calc R . . . .
C6 C 0.7602(3) 0.6457(2) 0.4494(6) 0.0394(12) Uani 1 1 d . . . . .
H6 H 0.7823 0.6102 0.4243 0.047 Uiso 1 1 calc R . . . .
C7 C 0.7987(3) 0.6950(2) 0.4034(6) 0.0344(11) Uani 1 1 d . . . . .
H7 H 0.8462 0.6923 0.3476 0.041 Uiso 1 1 calc R . . . .
C8 C 0.7674(3) 0.7500 0.4395(7) 0.0268(13) Uani 1 2 d S T P . .
C9 C 0.6956(3) 0.7500 0.5218(7) 0.0191(11) Uani 1 2 d S T P . .
C10 C 0.6550(2) 0.69970(17) 0.5692(5) 0.0227(8) Uani 1 1 d . . . . .
C11 C 0.5831(2) 0.71906(18) 0.6500(5) 0.0248(9) Uani 1 1 d . . . . .
C12 C 0.5208(3) 0.6891(2) 0.7181(6) 0.0363(11) Uani 1 1 d . . . . .
H12 H 0.5196 0.6490 0.7170 0.044 Uiso 1 1 calc R . . . .
C13 C 0.4601(3) 0.7208(3) 0.7885(6) 0.0481(15) Uani 1 1 d . . . . .
H13 H 0.4183 0.7014 0.8368 0.058 Uiso 1 1 calc R . . . .
C14 C 0.4304(4) 0.5087(3) 0.4349(9) 0.028(3) Uani 0.5 1 d . . . A -1
C15 C 0.3577(4) 0.5192(3) 0.3651(8) 0.031(2) Uani 0.5 1 d G . . A -1
H15 H 0.3460 0.5065 0.2542 0.037 Uiso 0.5 1 calc R . . A -1
C16 C 0.3024(3) 0.5486(3) 0.4611(11) 0.040(3) Uani 0.5 1 d G . . A -1
H16 H 0.2537 0.5556 0.4143 0.048 Uiso 0.5 1 calc R . . A -1
C17 C 0.3198(4) 0.5676(4) 0.6268(10) 0.052(4) Uani 0.5 1 d G . . A -1
H17 H 0.2828 0.5873 0.6910 0.063 Uiso 0.5 1 calc R . . A -1
C18 C 0.3925(4) 0.5571(3) 0.6967(8) 0.043(3) Uani 0.5 1 d G . . A -1
H18 H 0.4042 0.5698 0.8076 0.052 Uiso 0.5 1 calc R . . A -1
C19 C 0.4478(3) 0.5277(3) 0.6007(9) 0.0252(18) Uani 0.5 1 d G U . A -1
C20 C 0.5256(7) 0.5132(5) 0.6505(15) 0.019(2) Uani 0.5 1 d . . . A -1
C21 C 0.5773(6) 0.5179(3) 0.7882(13) 0.038(2) Uani 0.5 1 d . . . A -1
H21 H 0.5610 0.5357 0.8895 0.045 Uiso 0.5 1 calc R . . A -1
C22 C 0.6522(5) 0.4967(3) 0.7782(11) 0.0246(17) Uani 0.5 1 d . . . A -1
H22 H 0.6853 0.5006 0.8721 0.030 Uiso 0.5 1 calc R . . A -1
C23 C 0.6782(7) 0.4694(5) 0.6260(16) 0.035(3) Uani 0.5 1 d . . . A -1
H23 H 0.7287 0.4556 0.6224 0.042 Uiso 0.5 1 calc R . . A -1
C24 C 0.6299(4) 0.4619(3) 0.4762(9) 0.035(2) Uani 0.5 1 d . . . A -1
C25 C 0.6481(4) 0.4363(4) 0.3190(12) 0.059(5) Uani 0.5 1 d G . . A -1
H25 H 0.6971 0.4209 0.3012 0.071 Uiso 0.5 1 calc R . . A -1
C26 C 0.5930(5) 0.4337(4) 0.1886(9) 0.062(4) Uani 0.5 1 d G . . A -1
H26 H 0.6051 0.4165 0.0834 0.074 Uiso 0.5 1 calc R . . A -1
C27 C 0.5197(5) 0.4567(3) 0.2153(9) 0.063(4) Uani 0.5 1 d G . . A -1
H27 H 0.4829 0.4549 0.1280 0.076 Uiso 0.5 1 calc R . . A -1
C28 C 0.5016(4) 0.4823(4) 0.3724(10) 0.031(4) Uani 0.5 1 d G . . A -1
C29 C 0.5567(4) 0.4849(3) 0.5029(8) 0.020(2) Uani 0.5 1 d G . . A -1
F1 F 0.68020(16) 0.64898(11) 0.0476(3) 0.0354(6) Uani 1 1 d . . . . .
F2 F 0.47185(19) 0.7500 0.2845(5) 0.0289(8) Uani 1 2 d S T P . .
I1 I 0.79389(2) 0.7500 -0.06138(5) 0.03707(14) Uani 1 2 d S T P . .
I2 I 0.52070(2) 0.62088(2) 0.22803(4) 0.03852(13) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.019(3) 0.031(3) 0.014(2) 0.000 -0.003(2) 0.000
C2 0.028(2) 0.0176(17) 0.0181(18) -0.0047(14) -0.0083(16) 0.0079(15)
C3 0.027(2) 0.0160(17) 0.0210(18) 0.0004(14) -0.0083(16) -0.0049(15)
C4 0.021(3) 0.021(3) 0.019(3) 0.000 -0.003(2) 0.000
C5 0.042(3) 0.027(2) 0.025(2) 0.0048(17) -0.011(2) 0.0024(19)
C6 0.045(3) 0.040(3) 0.033(2) -0.007(2) -0.011(2) 0.023(2)
C7 0.021(2) 0.061(3) 0.021(2) -0.003(2) -0.0053(17) 0.018(2)
C8 0.018(3) 0.047(4) 0.015(3) 0.000 -0.007(2) 0.000
C9 0.012(2) 0.027(3) 0.018(3) 0.000 -0.008(2) 0.000
C10 0.025(2) 0.027(2) 0.0159(18) 0.0034(15) -0.0078(16) -0.0014(16)
C11 0.021(2) 0.036(2) 0.0176(18) 0.0046(16) -0.0049(16) -0.0038(17)
C12 0.030(2) 0.059(3) 0.019(2) 0.013(2) -0.0048(18) -0.012(2)
C13 0.020(2) 0.109(5) 0.015(2) 0.011(2) -0.0005(17) -0.008(2)
C14 0.037(6) 0.018(4) 0.029(7) 0.005(4) -0.013(5) -0.009(4)
C15 0.020(5) 0.020(4) 0.052(7) 0.004(4) 0.003(5) 0.005(4)
C16 0.034(6) 0.022(5) 0.063(8) 0.000(5) -0.007(5) 0.015(4)
C17 0.059(10) 0.042(7) 0.056(8) -0.004(6) 0.003(7) 0.021(6)
C18 0.048(8) 0.040(6) 0.042(6) -0.007(5) 0.010(6) 0.006(6)
C19 0.022(4) 0.008(3) 0.046(5) 0.009(4) -0.003(4) 0.004(3)
C20 0.028(6) 0.014(4) 0.015(4) 0.005(3) -0.006(4) -0.003(4)
C21 0.051(6) 0.014(4) 0.048(6) 0.016(4) 0.008(5) -0.006(4)
C22 0.030(4) 0.017(3) 0.028(4) 0.012(3) -0.005(4) -0.008(3)
C23 0.018(5) 0.028(5) 0.060(7) 0.015(5) 0.010(5) 0.007(4)
C24 0.038(5) 0.017(4) 0.051(6) 0.008(4) 0.012(5) 0.002(4)
C25 0.068(13) 0.033(7) 0.076(11) -0.015(7) 0.044(11) -0.011(7)
C26 0.053(8) 0.052(7) 0.081(10) -0.011(7) 0.022(8) -0.001(6)
C27 0.116(12) 0.027(5) 0.047(7) -0.007(5) 0.036(7) -0.023(6)
C28 0.054(11) 0.015(5) 0.023(6) 0.005(4) -0.014(6) -0.007(6)
C29 0.029(5) 0.012(4) 0.020(6) -0.002(4) 0.000(5) -0.004(3)
F1 0.0406(15) 0.0262(13) 0.0394(15) -0.0118(11) -0.0054(12) 0.0139(11)
F2 0.0171(16) 0.040(2) 0.0298(19) 0.000 -0.0004(14) 0.000
I1 0.0218(2) 0.0727(3) 0.0168(2) 0.000 0.00074(16) 0.000
I2 0.0483(2) 0.02120(15) 0.0461(2) 0.00941(12) -0.01689(15) -0.01624(12)
_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
C1 C2 1.376(5) 7_575 ?
C1 C2 1.376(5) . ?
C1 I1 2.082(6) . ?
C2 C3 1.384(6) . ?
C2 F1 1.338(4) . ?
C3 C4 1.380(5) . ?
C3 I2 2.072(4) . ?
C4 C3 1.380(5) 7_575 ?
C4 F2 1.337(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.417(7) . ?
C5 C10 1.366(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.371(8) . ?
C7 H7 0.9300 . ?
C7 C8 1.413(5) . ?
C8 C7 1.413(5) 7_575 ?
C8 C9 1.396(8) . ?
C9 C10 1.409(5) . ?
C9 C10 1.409(5) 7_575 ?
C10 C11 1.463(6) . ?
C11 C11 1.435(8) 7_575 ?
C11 C12 1.386(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.394(8) . ?
C13 C13 1.353(13) 7_575 ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 C19 1.3900 . ?
C14 C28 1.458(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.3900 . ?
C16 H16 0.9300 . ?
C16 C17 1.3900 . ?
C17 H17 0.9300 . ?
C17 C18 1.3900 . ?
C18 H18 0.9300 . ?
C18 C19 1.3900 . ?
C19 C20 1.439(12) . ?
C20 C21 1.395(16) . ?
C20 C29 1.423(12) . ?
C21 H21 0.9300 . ?
C21 C22 1.387(13) . ?
C22 H22 0.9300 . ?
C22 C23 1.412(16) . ?
C23 H23 0.9300 . ?
C23 C24 1.439(14) . ?
C24 C25 1.3900 . ?
C24 C29 1.3900 . ?
C25 H25 0.9300 . ?
C25 C26 1.3900 . ?
C26 H26 0.9300 . ?
C26 C27 1.3900 . ?
C27 H27 0.9300 . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
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
C2 C1 C2 117.7(5) 7_575 . ?
C2 C1 I1 121.1(3) 7_575 . ?
C2 C1 I1 121.1(3) . . ?
C1 C2 C3 122.5(4) . . ?
F1 C2 C1 119.4(4) . . ?
F1 C2 C3 118.1(4) . . ?
C2 C3 I2 121.8(3) . . ?
C4 C3 C2 117.6(4) . . ?
C4 C3 I2 120.7(3) . . ?
C3 C4 C3 122.3(5) 7_575 . ?
F2 C4 C3 118.8(3) . 7_575 ?
F2 C4 C3 118.8(3) . . ?
C6 C5 H5 120.7 . . ?
C10 C5 H5 120.7 . . ?
C10 C5 C6 118.7(4) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 C5 122.0(4) . . ?
C7 C6 H6 119.0 . . ?
C6 C7 H7 119.5 . . ?
C6 C7 C8 121.0(4) . . ?
C8 C7 H7 119.5 . . ?
C7 C8 C7 128.9(6) . 7_575 ?
C9 C8 C7 115.6(3) . 7_575 ?
C9 C8 C7 115.6(3) . . ?
C8 C9 C10 124.2(3) . 7_575 ?
C8 C9 C10 124.2(3) . . ?
C10 C9 C10 111.7(5) 7_575 . ?
C5 C10 C9 118.6(4) . . ?
C5 C10 C11 135.1(4) . . ?
C9 C10 C11 106.3(4) . . ?
C11 C11 C10 107.9(2) 7_575 . ?
C12 C11 C10 132.0(4) . . ?
C12 C11 C11 120.1(3) . 7_575 ?
C11 C12 H12 121.0 . . ?
C11 C12 C13 118.0(5) . . ?
C13 C12 H12 121.0 . . ?
C12 C13 H13 119.0 . . ?
C13 C13 C12 121.9(3) 7_575 . ?
C13 C13 H13 119.0 7_575 . ?
C15 C14 C19 120.0 . . ?
C15 C14 C28 135.1(6) . . ?
C19 C14 C28 104.9(6) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C17 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C14 C19 C20 112.1(7) . . ?
C18 C19 C14 120.0 . . ?
C18 C19 C20 127.9(7) . . ?
C21 C20 C19 141.7(12) . . ?
C21 C20 C29 114.1(11) . . ?
C29 C20 C19 104.2(8) . . ?
C20 C21 H21 119.1 . . ?
C22 C21 C20 121.9(10) . . ?
C22 C21 H21 119.1 . . ?
C21 C22 H22 119.9 . . ?
C21 C22 C23 120.2(9) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 118.6 . . ?
C22 C23 C24 122.8(10) . . ?
C24 C23 H23 118.6 . . ?
C25 C24 C23 128.8(7) . . ?
C25 C24 C29 120.0 . . ?
C29 C24 C23 111.2(7) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 120.0 . . ?
C25 C26 C27 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 C14 131.4(6) . . ?
C29 C28 C14 108.6(6) . . ?
C29 C28 C27 120.0 . . ?
C24 C29 C20 129.8(7) . . ?
C28 C29 C20 110.2(7) . . ?
C28 C29 C24 120.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0.0(6) . . . . ?
C1 C2 C3 I2 179.8(3) . . . . ?
C2 C1 C2 C3 -0.6(8) 7_575 . . . ?
C2 C1 C2 F1 177.8(3) 7_575 . . . ?
C2 C3 C4 C3 0.6(8) . . . 7_575 ?
C2 C3 C4 F2 179.7(4) . . . . ?
C5 C6 C7 C8 0.2(7) . . . . ?
C5 C10 C11 C11 179.4(4) . . . 7_575 ?
C5 C10 C11 C12 -1.2(8) . . . . ?
C6 C5 C10 C9 -0.9(6) . . . . ?
C6 C5 C10 C11 179.2(4) . . . . ?
C6 C7 C8 C7 179.5(4) . . . 7_575 ?
C6 C7 C8 C9 -0.6(7) . . . . ?
C7 C8 C9 C10 -179.8(4) 7_575 . . . ?
C7 C8 C9 C10 179.8(4) . . . 7_575 ?
C7 C8 C9 C10 0.3(8) . . . . ?
C7 C8 C9 C10 -0.3(8) 7_575 . . 7_575 ?
C8 C9 C10 C5 0.4(7) . . . . ?
C8 C9 C10 C11 -179.6(5) . . . . ?
C9 C10 C11 C11 -0.5(3) . . . 7_575 ?
C9 C10 C11 C12 178.8(4) . . . . ?
C10 C5 C6 C7 0.6(7) . . . . ?
C10 C9 C10 C5 -179.1(3) 7_575 . . . ?
C10 C9 C10 C11 0.9(6) 7_575 . . . ?
C10 C11 C12 C13 179.5(4) . . . . ?
C11 C11 C12 C13 -1.2(5) 7_575 . . . ?
C11 C12 C13 C13 1.3(5) . . . 7_575 ?
C14 C15 C16 C17 0.0 . . . . ?
C14 C19 C20 C21 -179.0(13) . . . . ?
C14 C19 C20 C29 1.3(9) . . . . ?
C14 C28 C29 C20 -1.1(8) . . . . ?
C14 C28 C29 C24 179.3(7) . . . . ?
C15 C14 C19 C18 0.0 . . . . ?
C15 C14 C19 C20 -179.7(7) . . . . ?
C15 C14 C28 C27 -1.7(10) . . . . ?
C15 C14 C28 C29 179.1(4) . . . . ?
C15 C16 C17 C18 0.0 . . . . ?
C16 C17 C18 C19 0.0 . . . . ?
C17 C18 C19 C14 0.0 . . . . ?
C17 C18 C19 C20 179.7(9) . . . . ?
C18 C19 C20 C21 1(2) . . . . ?
C18 C19 C20 C29 -178.4(4) . . . . ?
C19 C14 C15 C16 0.0 . . . . ?
C19 C14 C28 C27 -178.9(7) . . . . ?
C19 C14 C28 C29 1.8(5) . . . . ?
C19 C20 C21 C22 -179.3(13) . . . . ?
C19 C20 C29 C24 179.5(8) . . . . ?
C19 C20 C29 C28 0.0(10) . . . . ?
C20 C21 C22 C23 -0.1(13) . . . . ?
C21 C20 C29 C24 -0.3(10) . . . . ?
C21 C20 C29 C28 -179.8(7) . . . . ?
C21 C22 C23 C24 -0.1(13) . . . . ?
C22 C23 C24 C25 179.6(7) . . . . ?
C22 C23 C24 C29 0.1(11) . . . . ?
C23 C24 C25 C26 -179.5(8) . . . . ?
C23 C24 C29 C20 0.1(8) . . . . ?
C23 C24 C29 C28 179.6(7) . . . . ?
C24 C25 C26 C27 0.0 . . . . ?
C25 C24 C29 C20 -179.5(8) . . . . ?
C25 C24 C29 C28 0.0 . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C14 -179.1(9) . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C20 179.6(6) . . . . ?
C27 C28 C29 C24 0.0 . . . . ?
C28 C14 C15 C16 -177.0(7) . . . . ?
C28 C14 C19 C18 177.8(5) . . . . ?
C28 C14 C19 C20 -1.9(6) . . . . ?
C29 C20 C21 C22 0.3(13) . . . . ?
C29 C24 C25 C26 0.0 . . . . ?
F1 C2 C3 C4 -178.5(4) . . . . ?
F1 C2 C3 I2 1.4(5) . . . . ?
I1 C1 C2 C3 177.6(3) . . . . ?
I1 C1 C2 F1 -4.0(6) . . . . ?
I2 C3 C4 C3 -179.2(3) . . . 7_575 ?
I2 C3 C4 F2 -0.1(6) . . . . ?
_shelx_res_file
;
20161218e.res created by SHELXL-2014/7
TITL 20161218e_a.res in Pnma
CELL 0.71073 17.29279 23.187589 7.743108 90 90 90
ZERR 4 0.000859 0.000957 0.00038 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H F I
UNIT 152 80 12 12
ISOR 0.01 0.02 C19
L.S. 10
PLAN 3
BOND $H
CONF
MORE -1
fmap 2
acta 52
REM
REM
REM
WGHT 0.026800 14.487100
EXTI 0.003080
FVAR 0.20089
C1 1 0.684200 0.750000 0.049604 10.50000 0.01932 0.03133 =
0.01434 0.00000 -0.00266 0.00000
C2 1 0.647178 0.699230 0.089770 11.00000 0.02798 0.01758 =
0.01808 -0.00473 -0.00826 0.00787
C3 1 0.575507 0.697877 0.169285 11.00000 0.02667 0.01599 =
0.02098 0.00037 -0.00830 -0.00494
C4 1 0.541196 0.750000 0.208310 10.50000 0.02061 0.02110 =
0.01887 0.00000 -0.00328 0.00000
C5 1 0.687540 0.647317 0.534027 11.00000 0.04231 0.02665 =
0.02502 0.00477 -0.01075 0.00242
AFIX 43
H5 2 0.662513 0.613361 0.565044 11.00000 -1.20000
AFIX 0
C6 1 0.760174 0.645725 0.449377 11.00000 0.04541 0.04006 =
0.03280 -0.00661 -0.01114 0.02282
AFIX 43
H6 2 0.782337 0.610156 0.424277 11.00000 -1.20000
AFIX 0
C7 1 0.798738 0.695038 0.403390 11.00000 0.02131 0.06118 =
0.02086 -0.00309 -0.00527 0.01842
AFIX 43
H7 2 0.846224 0.692276 0.347619 11.00000 -1.20000
AFIX 0
C8 1 0.767390 0.750000 0.439491 10.50000 0.01784 0.04729 =
0.01534 0.00000 -0.00715 0.00000
C9 1 0.695572 0.750000 0.521830 10.50000 0.01216 0.02732 =
0.01792 0.00000 -0.00751 0.00000
C10 1 0.655016 0.699701 0.569161 11.00000 0.02535 0.02671 =
0.01594 0.00343 -0.00780 -0.00144
C11 1 0.583054 0.719059 0.649965 11.00000 0.02077 0.03604 =
0.01763 0.00460 -0.00493 -0.00384
C12 1 0.520802 0.689065 0.718149 11.00000 0.03049 0.05932 =
0.01909 0.01301 -0.00480 -0.01156
AFIX 43
H12 2 0.519603 0.648969 0.716992 11.00000 -1.20000
AFIX 0
C13 1 0.460068 0.720827 0.788485 11.00000 0.02007 0.10878 =
0.01537 0.01134 -0.00047 -0.00838
AFIX 43
H13 2 0.418332 0.701352 0.836820 11.00000 -1.20000
AFIX 66
PART -1
C14 1 0.430371 0.508696 0.434937 10.50000 0.03670 0.01764 =
0.02871 0.00548 -0.01307 -0.00852
C15 1 0.357664 0.519164 0.365113 10.50000 0.02002 0.01987 =
0.05249 0.00356 0.00279 0.00497
AFIX 43
H15 2 0.346006 0.506469 0.254197 10.50000 -1.20000
AFIX 65
C16 1 0.302380 0.548608 0.461066 10.50000 0.03396 0.02242 =
0.06315 0.00018 -0.00738 0.01453
AFIX 43
H16 2 0.253734 0.555612 0.414348 10.50000 -1.20000
AFIX 65
C17 1 0.319803 0.567583 0.626844 10.50000 0.05888 0.04159 =
0.05595 -0.00387 0.00328 0.02103
AFIX 43
H17 2 0.282814 0.587282 0.691043 10.50000 -1.20000
AFIX 65
C18 1 0.392510 0.557114 0.696671 10.50000 0.04822 0.04000 =
0.04172 -0.00694 0.00974 0.00569
AFIX 43
H18 2 0.404167 0.569809 0.807587 10.50000 -1.20000
AFIX 65
C19 1 0.447795 0.527671 0.600719 10.50000 0.02190 0.00775 =
0.04591 0.00905 -0.00291 0.00359
AFIX 0
C20 1 0.525616 0.513210 0.650476 10.50000 0.02795 0.01447 =
0.01518 0.00489 -0.00567 -0.00343
C21 1 0.577278 0.517910 0.788159 10.50000 0.05057 0.01437 =
0.04774 0.01568 0.00769 -0.00563
AFIX 43
H21 2 0.561042 0.535734 0.889460 10.50000 -1.20000
AFIX 0
C22 1 0.652175 0.496749 0.778218 10.50000 0.02976 0.01657 =
0.02756 0.01174 -0.00537 -0.00794
AFIX 43
H22 2 0.685345 0.500594 0.872054 10.50000 -1.20000
AFIX 0
C23 1 0.678196 0.469382 0.625981 10.50000 0.01796 0.02809 =
0.05985 0.01458 0.01017 0.00675
AFIX 43
H23 2 0.728677 0.455603 0.622375 10.50000 -1.20000
AFIX 66
C24 1 0.629948 0.461899 0.476175 10.50000 0.03818 0.01669 =
0.05138 0.00787 0.01186 0.00163
C25 1 0.648100 0.436273 0.319036 10.50000 0.06781 0.03263 =
0.07613 -0.01511 0.04411 -0.01118
AFIX 43
H25 2 0.697114 0.420879 0.301184 10.50000 -1.20000
AFIX 65
C26 1 0.592997 0.433654 0.188579 10.50000 0.05317 0.05170 =
0.08080 -0.01123 0.02190 -0.00131
AFIX 43
H26 2 0.605142 0.416508 0.083443 10.50000 -1.20000
AFIX 65
C27 1 0.519740 0.456661 0.215260 10.50000 0.11574 0.02682 =
0.04683 -0.00743 0.03594 -0.02331
AFIX 43
H27 2 0.482873 0.454909 0.127975 10.50000 -1.20000
AFIX 65
C28 1 0.501587 0.482288 0.372398 10.50000 0.05362 0.01528 =
0.02275 0.00534 -0.01412 -0.00658
C29 1 0.556690 0.484907 0.502856 10.50000 0.02928 0.01193 =
0.02025 -0.00220 0.00045 -0.00369
AFIX 0
PART 0
F1 3 0.680197 0.648976 0.047622 11.00000 0.04055 0.02622 =
0.03940 -0.01181 -0.00540 0.01388
F2 3 0.471847 0.750000 0.284503 10.50000 0.01714 0.03980 =
0.02985 0.00000 -0.00044 0.00000
I1 4 0.793893 0.750000 -0.061384 10.50000 0.02175 0.07266 =
0.01680 0.00000 0.00074 0.00000
I2 4 0.520702 0.620884 0.228032 11.00000 0.04827 0.02120 =
0.04608 0.00941 -0.01689 -0.01624
HKLF 4
REM 20161218e_a.res in Pnma
REM R1 = 0.0430 for 3428 Fo > 4sig(Fo) and 0.0568 for all 4188 data
REM 257 parameters refined using 6 restraints
END
WGHT 0.0268 14.4867
REM Highest difference peak 1.986, deepest hole -2.422, 1-sigma level 0.139
Q1 1 0.5607 0.6106 0.2192 11.00000 0.05 1.99
Q2 1 0.5065 0.6322 0.3088 11.00000 0.05 1.62
Q3 1 0.5021 0.6169 0.1714 11.00000 0.05 1.28
;
_shelx_res_checksum 20367
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.092
_oxdiff_exptl_absorpt_empirical_full_min 0.865
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_20161127c
_database_code_depnum_ccdc_archive 'CCDC 1547625'
_audit_update_record
;
2017-06-30 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_audit_creation_date 2016-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common ?
_chemical_name_systematic FA
_chemical_formula_moiety 'C16 H10'
_chemical_formula_sum 'C16 H10'
_chemical_formula_weight 202.24
_chemical_melting_point ?
_chemical_oxdiff_formula c1h1f1i1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 17.8455(8)
_cell_length_b 6.2494(3)
_cell_length_c 19.5446(10)
_cell_angle_alpha 90
_cell_angle_beta 108.407(5)
_cell_angle_gamma 90
_cell_volume 2068.17(18)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 4138
_cell_measurement_temperature 100.01(10)
_cell_measurement_theta_max 29.1550
_cell_measurement_theta_min 3.7580
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.074
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.91635
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_density_diffrn 1.299
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 848
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.25
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0243
_diffrn_reflns_av_unetI/netI 0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 11278
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 29.827
_diffrn_reflns_theta_min 3.425
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -10.00 87.00 1.00 10.00 -- 12.76 37.00 120.00 97
2 \w 58.00 84.00 1.00 10.00 -- 12.76 37.00 150.00 26
3 \w -45.00 46.00 1.00 10.00 -- 12.76 -19.00 -60.00 91
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0182986000
_diffrn_orient_matrix_UB_12 -0.0058685000
_diffrn_orient_matrix_UB_13 -0.0378465000
_diffrn_orient_matrix_UB_21 -0.0352908000
_diffrn_orient_matrix_UB_22 0.0425620000
_diffrn_orient_matrix_UB_23 0.0039013000
_diffrn_orient_matrix_UB_31 0.0132768000
_diffrn_orient_matrix_UB_32 0.1050596000
_diffrn_orient_matrix_UB_33 -0.0036937000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4073
_reflns_number_total 4993
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.267
_refine_diff_density_min -0.268
_refine_diff_density_rms 0.048
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 289
_refine_ls_number_reflns 4993
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0625
_refine_ls_R_factor_gt 0.0491
_refine_ls_restrained_S_all 1.026
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+0.8772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1101
_refine_ls_wR_factor_ref 0.1185
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C25(H25), C26(H26),
C28(H28), C29(H29), C30(H30)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
C1 C 0.46661(8) 0.0557(2) 0.86828(8) 0.0218(3) Uani 1 1 d . . . . .
H1 H 0.4966 -0.0690 0.8769 0.026 Uiso 1 1 calc R . . . .
C2 C 0.47260(9) 0.2023(2) 0.92359(8) 0.0251(3) Uani 1 1 d . . . . .
H2 H 0.5071 0.1749 0.9695 0.030 Uiso 1 1 calc R . . . .
C3 C 0.42773(9) 0.3892(2) 0.91106(8) 0.0235(3) Uani 1 1 d . . . . .
H3 H 0.4328 0.4848 0.9487 0.028 Uiso 1 1 calc R . . . .
C4 C 0.37533(8) 0.4349(2) 0.84288(7) 0.0212(3) Uani 1 1 d . . . . .
H4 H 0.3454 0.5598 0.8347 0.025 Uiso 1 1 calc R . . . .
C5 C 0.36886(8) 0.2898(2) 0.78756(7) 0.0179(3) Uani 1 1 d . . . . .
C6 C 0.41498(8) 0.1001(2) 0.80017(7) 0.0182(3) Uani 1 1 d . . . . .
C7 C 0.39608(8) -0.0189(2) 0.73130(7) 0.0181(3) Uani 1 1 d . . . . .
C8 C 0.42307(8) -0.2026(2) 0.70865(8) 0.0213(3) Uani 1 1 d . . . . .
H8 H 0.4611 -0.2869 0.7409 0.026 Uiso 1 1 calc R . . . .
C9 C 0.39190(9) -0.2614(2) 0.63507(8) 0.0226(3) Uani 1 1 d . . . . .
H9 H 0.4106 -0.3850 0.6195 0.027 Uiso 1 1 calc R . . . .
C10 C 0.33490(8) -0.1425(2) 0.58568(8) 0.0214(3) Uani 1 1 d . . . . .
H10 H 0.3155 -0.1875 0.5380 0.026 Uiso 1 1 calc R . . . .
C11 C 0.30561(8) 0.0490(2) 0.60749(7) 0.0189(3) Uani 1 1 d . . . . .
C12 C 0.24749(8) 0.1926(2) 0.56471(7) 0.0206(3) Uani 1 1 d . . . . .
H12 H 0.2232 0.1643 0.5160 0.025 Uiso 1 1 calc R . . . .
C13 C 0.22726(8) 0.3730(2) 0.59529(8) 0.0216(3) Uani 1 1 d . . . . .
H13 H 0.1886 0.4631 0.5665 0.026 Uiso 1 1 calc R . . . .
C14 C 0.26294(8) 0.4272(2) 0.66898(8) 0.0206(3) Uani 1 1 d . . . . .
H14 H 0.2487 0.5514 0.6880 0.025 Uiso 1 1 calc R . . . .
C15 C 0.31886(8) 0.2917(2) 0.71131(7) 0.0178(3) Uani 1 1 d . . . . .
C16 C 0.33828(8) 0.1038(2) 0.67999(7) 0.0169(3) Uani 1 1 d . . . . .
C17 C 0.60968(9) 0.5441(2) 0.86013(8) 0.0248(3) Uani 1 1 d . . . . .
H17 H 0.5845 0.4205 0.8679 0.030 Uiso 1 1 calc R . . . .
C18 C 0.64122(9) 0.6900(3) 0.91587(8) 0.0283(3) Uani 1 1 d . . . . .
H18 H 0.6369 0.6631 0.9613 0.034 Uiso 1 1 calc R . . . .
C19 C 0.67894(9) 0.8747(3) 0.90464(8) 0.0266(3) Uani 1 1 d . . . . .
H19 H 0.6997 0.9691 0.9427 0.032 Uiso 1 1 calc R . . . .
C20 C 0.68619(8) 0.9208(2) 0.83732(8) 0.0223(3) Uani 1 1 d . . . . .
H20 H 0.7112 1.0452 0.8300 0.027 Uiso 1 1 calc R . . . .
C21 C 0.65529(8) 0.7772(2) 0.78153(7) 0.0183(3) Uani 1 1 d . . . . .
C22 C 0.61675(8) 0.5877(2) 0.79272(7) 0.0192(3) Uani 1 1 d . . . . .
C23 C 0.58991(8) 0.4688(2) 0.72385(7) 0.0194(3) Uani 1 1 d . . . . .
C24 C 0.54784(8) 0.2849(2) 0.70006(8) 0.0249(3) Uani 1 1 d . . . . .
H24 H 0.5307 0.2008 0.7314 0.030 Uiso 1 1 calc R . . . .
C25 C 0.53107(9) 0.2257(2) 0.62694(9) 0.0278(3) Uani 1 1 d . . . . .
H25 H 0.5017 0.1024 0.6106 0.033 Uiso 1 1 calc R . . . .
C26 C 0.55652(8) 0.3435(2) 0.57897(8) 0.0261(3) Uani 1 1 d . . . . .
H26 H 0.5450 0.2977 0.5315 0.031 Uiso 1 1 calc R . . . .
C27 C 0.60032(8) 0.5346(2) 0.60170(8) 0.0220(3) Uani 1 1 d . . . . .
C28 C 0.63108(8) 0.6778(3) 0.56058(8) 0.0245(3) Uani 1 1 d . . . . .
H28 H 0.6241 0.6484 0.5123 0.029 Uiso 1 1 calc R . . . .
C29 C 0.67097(8) 0.8591(2) 0.59170(8) 0.0245(3) Uani 1 1 d . . . . .
H29 H 0.6907 0.9494 0.5637 0.029 Uiso 1 1 calc R . . . .
C30 C 0.68323(8) 0.9141(2) 0.66476(8) 0.0214(3) Uani 1 1 d . . . . .
H30 H 0.7098 1.0390 0.6842 0.026 Uiso 1 1 calc R . . . .
C31 C 0.65497(8) 0.7786(2) 0.70606(7) 0.0181(3) Uani 1 1 d . . . . .
C32 C 0.61473(8) 0.5911(2) 0.67388(7) 0.0186(3) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0196(7) 0.0225(7) 0.0232(7) 0.0045(5) 0.0065(5) -0.0018(6)
C2 0.0252(7) 0.0302(8) 0.0185(7) 0.0026(6) 0.0050(6) -0.0049(7)
C3 0.0260(7) 0.0277(8) 0.0189(7) -0.0030(6) 0.0100(6) -0.0058(7)
C4 0.0227(7) 0.0213(7) 0.0227(7) -0.0005(5) 0.0115(6) -0.0013(6)
C5 0.0171(6) 0.0198(7) 0.0188(7) 0.0017(5) 0.0087(5) -0.0025(6)
C6 0.0162(6) 0.0195(7) 0.0209(7) 0.0018(5) 0.0086(5) -0.0026(6)
C7 0.0166(6) 0.0190(7) 0.0202(7) 0.0016(5) 0.0079(5) -0.0032(6)
C8 0.0184(7) 0.0192(7) 0.0269(8) 0.0019(6) 0.0082(6) -0.0002(6)
C9 0.0258(7) 0.0169(7) 0.0284(8) -0.0032(5) 0.0134(6) -0.0010(6)
C10 0.0253(7) 0.0207(7) 0.0204(7) -0.0026(5) 0.0104(6) -0.0054(6)
C11 0.0197(7) 0.0197(7) 0.0198(7) 0.0016(5) 0.0098(5) -0.0041(6)
C12 0.0210(7) 0.0247(7) 0.0166(7) 0.0034(5) 0.0067(5) -0.0034(6)
C13 0.0201(7) 0.0227(7) 0.0226(7) 0.0077(5) 0.0076(6) 0.0028(6)
C14 0.0205(7) 0.0202(7) 0.0240(7) 0.0024(5) 0.0113(6) 0.0016(6)
C15 0.0174(6) 0.0191(7) 0.0201(7) 0.0009(5) 0.0101(5) -0.0023(6)
C16 0.0170(6) 0.0166(6) 0.0190(7) 0.0014(5) 0.0083(5) -0.0020(6)
C17 0.0223(7) 0.0279(8) 0.0273(8) 0.0095(6) 0.0122(6) 0.0061(6)
C18 0.0279(8) 0.0402(9) 0.0191(7) 0.0079(6) 0.0109(6) 0.0117(7)
C19 0.0245(7) 0.0332(8) 0.0206(7) -0.0029(6) 0.0047(6) 0.0064(7)
C20 0.0186(7) 0.0247(7) 0.0224(7) -0.0005(6) 0.0048(5) 0.0022(6)
C21 0.0141(6) 0.0215(7) 0.0188(7) 0.0027(5) 0.0046(5) 0.0040(6)
C22 0.0142(6) 0.0220(7) 0.0220(7) 0.0043(5) 0.0065(5) 0.0051(6)
C23 0.0148(6) 0.0204(7) 0.0238(7) 0.0039(5) 0.0073(5) 0.0035(6)
C24 0.0190(7) 0.0221(7) 0.0347(8) 0.0045(6) 0.0102(6) 0.0009(6)
C25 0.0198(7) 0.0209(7) 0.0383(9) -0.0046(6) 0.0030(6) -0.0018(6)
C26 0.0200(7) 0.0289(8) 0.0247(8) -0.0066(6) 0.0003(6) 0.0041(7)
C27 0.0161(6) 0.0260(7) 0.0219(7) -0.0007(6) 0.0034(5) 0.0037(6)
C28 0.0213(7) 0.0347(8) 0.0173(7) 0.0012(6) 0.0058(5) 0.0056(7)
C29 0.0219(7) 0.0306(8) 0.0232(7) 0.0087(6) 0.0101(6) 0.0031(7)
C30 0.0187(7) 0.0213(7) 0.0248(7) 0.0022(5) 0.0076(6) -0.0004(6)
C31 0.0136(6) 0.0208(7) 0.0190(7) 0.0023(5) 0.0040(5) 0.0028(6)
C32 0.0135(6) 0.0209(7) 0.0209(7) 0.0024(5) 0.0048(5) 0.0025(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9300 . ?
C1 C2 1.395(2) . ?
C1 C6 1.3867(19) . ?
C2 H2 0.9300 . ?
C2 C3 1.393(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.395(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.3879(19) . ?
C5 C6 1.4197(19) . ?
C5 C15 1.4757(19) . ?
C6 C7 1.4803(19) . ?
C7 C8 1.3716(19) . ?
C7 C16 1.4157(19) . ?
C8 H8 0.9300 . ?
C8 C9 1.417(2) . ?
C9 H9 0.9300 . ?
C9 C10 1.378(2) . ?
C10 H10 0.9300 . ?
C10 C11 1.4244(19) . ?
C11 C12 1.4254(19) . ?
C11 C16 1.3940(19) . ?
C12 H12 0.9300 . ?
C12 C13 1.377(2) . ?
C13 H13 0.9300 . ?
C13 C14 1.420(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.3696(19) . ?
C15 C16 1.4166(18) . ?
C17 H17 0.9300 . ?
C17 C18 1.396(2) . ?
C17 C22 1.3896(19) . ?
C18 H18 0.9300 . ?
C18 C19 1.388(2) . ?
C19 H19 0.9300 . ?
C19 C20 1.392(2) . ?
C20 H20 0.9300 . ?
C20 C21 1.3851(19) . ?
C21 C22 1.4207(19) . ?
C21 C31 1.4732(19) . ?
C22 C23 1.478(2) . ?
C23 C24 1.371(2) . ?
C23 C32 1.4169(19) . ?
C24 H24 0.9300 . ?
C24 C25 1.414(2) . ?
C25 H25 0.9300 . ?
C25 C26 1.377(2) . ?
C26 H26 0.9300 . ?
C26 C27 1.420(2) . ?
C27 C28 1.424(2) . ?
C27 C32 1.3969(19) . ?
C28 H28 0.9300 . ?
C28 C29 1.373(2) . ?
C29 H29 0.9300 . ?
C29 C30 1.417(2) . ?
C30 H30 0.9300 . ?
C30 C31 1.3711(19) . ?
C31 C32 1.4143(19) . ?
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
C2 C1 H1 120.7 . . ?
C6 C1 H1 120.7 . . ?
C6 C1 C2 118.53(14) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 C1 121.01(14) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 120.96(13) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 120.8 . . ?
C5 C4 C3 118.44(13) . . ?
C5 C4 H4 120.8 . . ?
C4 C5 C6 120.63(13) . . ?
C4 C5 C15 131.03(13) . . ?
C6 C5 C15 108.34(12) . . ?
C1 C6 C5 120.43(13) . . ?
C1 C6 C7 131.61(13) . . ?
C5 C6 C7 107.95(12) . . ?
C8 C7 C6 135.35(13) . . ?
C8 C7 C16 118.45(13) . . ?
C16 C7 C6 106.15(12) . . ?
C7 C8 H8 120.7 . . ?
C7 C8 C9 118.64(13) . . ?
C9 C8 H8 120.7 . . ?
C8 C9 H9 118.7 . . ?
C10 C9 C8 122.53(13) . . ?
C10 C9 H9 118.7 . . ?
C9 C10 H10 119.9 . . ?
C9 C10 C11 120.20(13) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C12 128.40(13) . . ?
C16 C11 C10 115.82(12) . . ?
C16 C11 C12 115.78(12) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.18(13) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 118.6 . . ?
C12 C13 C14 122.74(13) . . ?
C14 C13 H13 118.6 . . ?
C13 C14 H14 120.9 . . ?
C15 C14 C13 118.24(13) . . ?
C15 C14 H14 120.9 . . ?
C14 C15 C5 135.07(13) . . ?
C14 C15 C16 118.83(13) . . ?
C16 C15 C5 106.10(11) . . ?
C7 C16 C15 111.45(12) . . ?
C11 C16 C7 124.35(13) . . ?
C11 C16 C15 124.19(12) . . ?
C18 C17 H17 120.8 . . ?
C22 C17 H17 120.8 . . ?
C22 C17 C18 118.48(14) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 121.08(14) . . ?
C19 C18 H18 119.5 . . ?
C18 C19 H19 119.5 . . ?
C18 C19 C20 121.06(14) . . ?
C20 C19 H19 119.5 . . ?
C19 C20 H20 120.7 . . ?
C21 C20 C19 118.51(14) . . ?
C21 C20 H20 120.7 . . ?
C20 C21 C22 120.70(13) . . ?
C20 C21 C31 131.22(13) . . ?
C22 C21 C31 108.08(12) . . ?
C17 C22 C21 120.18(13) . . ?
C17 C22 C23 131.63(13) . . ?
C21 C22 C23 108.19(12) . . ?
C24 C23 C22 135.66(13) . . ?
C24 C23 C32 118.37(13) . . ?
C32 C23 C22 105.94(12) . . ?
C23 C24 H24 120.6 . . ?
C23 C24 C25 118.72(14) . . ?
C25 C24 H24 120.6 . . ?
C24 C25 H25 118.7 . . ?
C26 C25 C24 122.57(14) . . ?
C26 C25 H25 118.7 . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C27 120.27(14) . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C28 128.64(14) . . ?
C32 C27 C26 115.85(13) . . ?
C32 C27 C28 115.50(13) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 C27 120.45(13) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 H29 118.7 . . ?
C28 C29 C30 122.68(13) . . ?
C30 C29 H29 118.7 . . ?
C29 C30 H30 120.8 . . ?
C31 C30 C29 118.37(13) . . ?
C31 C30 H30 120.8 . . ?
C30 C31 C21 135.03(13) . . ?
C30 C31 C32 118.64(13) . . ?
C32 C31 C21 106.33(12) . . ?
C27 C32 C23 124.20(13) . . ?
C27 C32 C31 124.34(13) . . ?
C31 C32 C23 111.45(12) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0.2(2) . . . . ?
C1 C6 C7 C8 -3.4(3) . . . . ?
C1 C6 C7 C16 179.53(14) . . . . ?
C2 C1 C6 C5 -0.6(2) . . . . ?
C2 C1 C6 C7 179.14(14) . . . . ?
C2 C3 C4 C5 0.0(2) . . . . ?
C3 C4 C5 C6 -0.4(2) . . . . ?
C3 C4 C5 C15 179.12(13) . . . . ?
C4 C5 C6 C1 0.8(2) . . . . ?
C4 C5 C6 C7 -179.05(12) . . . . ?
C4 C5 C15 C14 -0.7(3) . . . . ?
C4 C5 C15 C16 178.99(14) . . . . ?
C5 C6 C7 C8 176.40(15) . . . . ?
C5 C6 C7 C16 -0.70(14) . . . . ?
C5 C15 C16 C7 1.00(15) . . . . ?
C5 C15 C16 C11 -177.88(12) . . . . ?
C6 C1 C2 C3 0.2(2) . . . . ?
C6 C5 C15 C14 178.85(15) . . . . ?
C6 C5 C15 C16 -1.42(14) . . . . ?
C6 C7 C8 C9 -176.88(14) . . . . ?
C6 C7 C16 C11 178.66(12) . . . . ?
C6 C7 C16 C15 -0.21(15) . . . . ?
C7 C8 C9 C10 -0.8(2) . . . . ?
C8 C7 C16 C11 1.0(2) . . . . ?
C8 C7 C16 C15 -177.89(12) . . . . ?
C8 C9 C10 C11 0.8(2) . . . . ?
C9 C10 C11 C12 179.78(14) . . . . ?
C9 C10 C11 C16 0.10(19) . . . . ?
C10 C11 C12 C13 -179.15(13) . . . . ?
C10 C11 C16 C7 -0.99(19) . . . . ?
C10 C11 C16 C15 177.74(12) . . . . ?
C11 C12 C13 C14 1.0(2) . . . . ?
C12 C11 C16 C7 179.29(12) . . . . ?
C12 C11 C16 C15 -1.98(19) . . . . ?
C12 C13 C14 C15 -1.1(2) . . . . ?
C13 C14 C15 C5 179.40(14) . . . . ?
C13 C14 C15 C16 -0.31(19) . . . . ?
C14 C15 C16 C7 -179.22(12) . . . . ?
C14 C15 C16 C11 1.9(2) . . . . ?
C15 C5 C6 C1 -178.89(12) . . . . ?
C15 C5 C6 C7 1.31(14) . . . . ?
C16 C7 C8 C9 -0.05(19) . . . . ?
C16 C11 C12 C13 0.53(19) . . . . ?
C17 C18 C19 C20 0.3(2) . . . . ?
C17 C22 C23 C24 2.7(3) . . . . ?
C17 C22 C23 C32 -179.50(14) . . . . ?
C18 C17 C22 C21 -0.1(2) . . . . ?
C18 C17 C22 C23 -179.62(14) . . . . ?
C18 C19 C20 C21 -0.4(2) . . . . ?
C19 C20 C21 C22 0.3(2) . . . . ?
C19 C20 C21 C31 -178.65(13) . . . . ?
C20 C21 C22 C17 0.0(2) . . . . ?
C20 C21 C22 C23 179.60(12) . . . . ?
C20 C21 C31 C30 -0.1(3) . . . . ?
C20 C21 C31 C32 -179.86(14) . . . . ?
C21 C22 C23 C24 -176.92(15) . . . . ?
C21 C22 C23 C32 0.91(15) . . . . ?
C21 C31 C32 C23 -0.53(15) . . . . ?
C21 C31 C32 C27 178.71(13) . . . . ?
C22 C17 C18 C19 -0.1(2) . . . . ?
C22 C21 C31 C30 -179.13(15) . . . . ?
C22 C21 C31 C32 1.10(14) . . . . ?
C22 C23 C24 C25 177.57(15) . . . . ?
C22 C23 C32 C27 -179.45(12) . . . . ?
C22 C23 C32 C31 -0.21(15) . . . . ?
C23 C24 C25 C26 1.2(2) . . . . ?
C24 C23 C32 C27 -1.2(2) . . . . ?
C24 C23 C32 C31 178.06(12) . . . . ?
C24 C25 C26 C27 -1.1(2) . . . . ?
C25 C26 C27 C28 -179.56(14) . . . . ?
C25 C26 C27 C32 -0.1(2) . . . . ?
C26 C27 C28 C29 178.59(14) . . . . ?
C26 C27 C32 C23 1.3(2) . . . . ?
C26 C27 C32 C31 -177.89(13) . . . . ?
C27 C28 C29 C30 -0.4(2) . . . . ?
C28 C27 C32 C23 -179.24(13) . . . . ?
C28 C27 C32 C31 1.6(2) . . . . ?
C28 C29 C30 C31 1.0(2) . . . . ?
C29 C30 C31 C21 -179.97(14) . . . . ?
C29 C30 C31 C32 -0.2(2) . . . . ?
C30 C31 C32 C23 179.65(12) . . . . ?
C30 C31 C32 C27 -1.1(2) . . . . ?
C31 C21 C22 C17 179.11(12) . . . . ?
C31 C21 C22 C23 -1.24(14) . . . . ?
C32 C23 C24 C25 0.0(2) . . . . ?
C32 C27 C28 C29 -0.8(2) . . . . ?
_shelx_res_file
;
20161127c.res created by SHELXL-2014/7
TITL 20161127c_a.res in P2(1)/n
REM Old TITL 20161127c in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.126, Rweak 0.242, Alpha 0.026, Orientation as input
REM Formula found by SHELXT: C21
CELL 0.71073 17.845534 6.249382 19.544647 90 108.4072 90
ZERR 8 0.000845 0.000263 0.001009 0 0.0052 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H
UNIT 128 80
L.S. 5
PLAN 5
BOND $H
MORE -1
CONF
fmap 2
acta 52
REM
REM
REM
WGHT 0.045500 0.877200
FVAR 0.44148
C1 1 0.466610 0.055711 0.868279 11.00000 0.01964 0.02247 =
0.02318 0.00455 0.00646 -0.00184
AFIX 43
H1 2 0.496577 -0.069002 0.876895 11.00000 -1.20000
AFIX 0
C2 1 0.472604 0.202340 0.923592 11.00000 0.02517 0.03020 =
0.01848 0.00262 0.00501 -0.00487
AFIX 43
H2 2 0.507076 0.174918 0.969522 11.00000 -1.20000
AFIX 0
C3 1 0.427734 0.389209 0.911063 11.00000 0.02598 0.02767 =
0.01889 -0.00298 0.00996 -0.00582
AFIX 43
H3 2 0.432799 0.484846 0.948715 11.00000 -1.20000
AFIX 0
C4 1 0.375333 0.434930 0.842877 11.00000 0.02274 0.02127 =
0.02265 -0.00053 0.01150 -0.00125
AFIX 43
H4 2 0.345432 0.559753 0.834666 11.00000 -1.20000
AFIX 0
C5 1 0.368860 0.289758 0.787563 11.00000 0.01708 0.01980 =
0.01884 0.00172 0.00866 -0.00251
C6 1 0.414981 0.100054 0.800173 11.00000 0.01615 0.01953 =
0.02086 0.00177 0.00856 -0.00264
C7 1 0.396082 -0.018857 0.731297 11.00000 0.01658 0.01901 =
0.02021 0.00164 0.00790 -0.00316
C8 1 0.423072 -0.202619 0.708649 11.00000 0.01840 0.01917 =
0.02695 0.00193 0.00818 -0.00018
AFIX 43
H8 2 0.461056 -0.286901 0.740932 11.00000 -1.20000
AFIX 0
C9 1 0.391901 -0.261411 0.635067 11.00000 0.02578 0.01695 =
0.02844 -0.00321 0.01336 -0.00104
AFIX 43
H9 2 0.410636 -0.384991 0.619509 11.00000 -1.20000
AFIX 0
C10 1 0.334901 -0.142540 0.585678 11.00000 0.02528 0.02067 =
0.02037 -0.00258 0.01039 -0.00544
AFIX 43
H10 2 0.315490 -0.187519 0.537956 11.00000 -1.20000
AFIX 0
C11 1 0.305613 0.049043 0.607487 11.00000 0.01970 0.01972 =
0.01981 0.00160 0.00980 -0.00409
C12 1 0.247491 0.192566 0.564710 11.00000 0.02104 0.02467 =
0.01663 0.00341 0.00666 -0.00340
AFIX 43
H12 2 0.223168 0.164252 0.516006 11.00000 -1.20000
AFIX 0
C13 1 0.227263 0.372976 0.595293 11.00000 0.02009 0.02266 =
0.02255 0.00766 0.00758 0.00280
AFIX 43
H13 2 0.188610 0.463107 0.566479 11.00000 -1.20000
AFIX 0
C14 1 0.262944 0.427177 0.668979 11.00000 0.02048 0.02024 =
0.02396 0.00240 0.01131 0.00160
AFIX 43
H14 2 0.248728 0.551399 0.688006 11.00000 -1.20000
AFIX 0
C15 1 0.318861 0.291683 0.711308 11.00000 0.01737 0.01906 =
0.02006 0.00086 0.01011 -0.00229
C16 1 0.338277 0.103836 0.679988 11.00000 0.01696 0.01656 =
0.01902 0.00145 0.00833 -0.00198
C17 1 0.609675 0.544097 0.860132 11.00000 0.02231 0.02788 =
0.02726 0.00949 0.01221 0.00607
AFIX 43
H17 2 0.584493 0.420518 0.867932 11.00000 -1.20000
AFIX 0
C18 1 0.641225 0.690046 0.915865 11.00000 0.02793 0.04018 =
0.01913 0.00785 0.01094 0.01168
AFIX 43
H18 2 0.636900 0.663116 0.961266 11.00000 -1.20000
AFIX 0
C19 1 0.678938 0.874670 0.904641 11.00000 0.02447 0.03316 =
0.02061 -0.00291 0.00469 0.00636
AFIX 43
H19 2 0.699700 0.969132 0.942694 11.00000 -1.20000
AFIX 0
C20 1 0.686191 0.920759 0.837322 11.00000 0.01860 0.02474 =
0.02244 -0.00052 0.00479 0.00219
AFIX 43
H20 2 0.711220 1.045155 0.829981 11.00000 -1.20000
AFIX 0
C21 1 0.655293 0.777179 0.781529 11.00000 0.01409 0.02154 =
0.01881 0.00275 0.00455 0.00400
C22 1 0.616753 0.587666 0.792721 11.00000 0.01423 0.02195 =
0.02196 0.00425 0.00650 0.00511
C23 1 0.589909 0.468785 0.723855 11.00000 0.01484 0.02038 =
0.02380 0.00386 0.00725 0.00353
C24 1 0.547839 0.284912 0.700065 11.00000 0.01900 0.02208 =
0.03473 0.00447 0.01016 0.00090
AFIX 43
H24 2 0.530662 0.200751 0.731424 11.00000 -1.20000
AFIX 0
C25 1 0.531073 0.225711 0.626941 11.00000 0.01976 0.02092 =
0.03827 -0.00457 0.00297 -0.00181
AFIX 43
H25 2 0.501713 0.102378 0.610600 11.00000 -1.20000
AFIX 0
C26 1 0.556518 0.343537 0.578967 11.00000 0.01999 0.02891 =
0.02466 -0.00656 0.00031 0.00410
AFIX 43
H26 2 0.544960 0.297732 0.531483 11.00000 -1.20000
AFIX 0
C27 1 0.600322 0.534640 0.601702 11.00000 0.01612 0.02603 =
0.02191 -0.00072 0.00336 0.00373
C28 1 0.631083 0.677830 0.560584 11.00000 0.02128 0.03467 =
0.01727 0.00123 0.00584 0.00559
AFIX 43
H28 2 0.624124 0.648440 0.512323 11.00000 -1.20000
AFIX 0
C29 1 0.670967 0.859075 0.591704 11.00000 0.02193 0.03056 =
0.02323 0.00868 0.01014 0.00305
AFIX 43
H29 2 0.690729 0.949391 0.563680 11.00000 -1.20000
AFIX 0
C30 1 0.683234 0.914082 0.664756 11.00000 0.01868 0.02134 =
0.02480 0.00215 0.00756 -0.00038
AFIX 43
H30 2 0.709803 1.038995 0.684211 11.00000 -1.20000
AFIX 0
C31 1 0.654974 0.778632 0.706064 11.00000 0.01355 0.02081 =
0.01903 0.00233 0.00400 0.00277
C32 1 0.614725 0.591074 0.673877 11.00000 0.01346 0.02086 =
0.02089 0.00237 0.00479 0.00250
HKLF 4
REM 20161127c_a.res in P2(1)/n
REM R1 = 0.0491 for 4073 Fo > 4sig(Fo) and 0.0625 for all 4993 data
REM 289 parameters refined using 0 restraints
END
WGHT 0.0455 0.8774
REM Highest difference peak 0.267, deepest hole -0.268, 1-sigma level 0.048
Q1 1 0.3340 0.2208 0.6906 11.00000 0.05 0.27
Q2 1 0.5859 0.5543 0.6894 11.00000 0.05 0.25
Q3 1 0.3432 0.3063 0.7491 11.00000 0.05 0.24
Q4 1 0.3229 -0.0406 0.5941 11.00000 0.05 0.24
Q5 1 0.4040 0.0084 0.7699 11.00000 0.05 0.22
;
_shelx_res_checksum 70269
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.146
_oxdiff_exptl_absorpt_empirical_full_min 0.738
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_20161218b
_database_code_depnum_ccdc_archive 'CCDC 1547630'
_audit_update_record
;
2017-07-20 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_audit_creation_date 2016-12-31
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common ?
_chemical_name_systematic 1IPB-FA
_chemical_formula_moiety 'C6 F5 I, C16 H10'
_chemical_formula_sum 'C22 H10 F5 I'
_chemical_formula_weight 496.20
_chemical_melting_point ?
_chemical_oxdiff_formula c1h1f1i1
_chemical_oxdiff_usercomment Eu
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 9.5860(6)
_cell_length_b 15.0356(7)
_cell_length_c 12.5798(6)
_cell_angle_alpha 90
_cell_angle_beta 105.274(5)
_cell_angle_gamma 90
_cell_volume 1749.09(16)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 2966
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 28.0090
_cell_measurement_theta_min 4.0930
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.886
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.51416
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.884
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description cube
_exptl_crystal_F_000 960
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.2
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0395
_diffrn_reflns_av_unetI/netI 0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 9526
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 29.950
_diffrn_reflns_theta_min 3.385
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -41.00 19.00 1.00 2.00 -- 12.76 -37.00 -60.00 60
2 \w -74.00 48.00 1.00 2.00 -- 12.76 0.00-180.00 122
3 \w 68.00 99.00 1.00 2.00 -- 12.76-178.00 -30.00 31
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0719132000
_diffrn_orient_matrix_UB_12 -0.0159231000
_diffrn_orient_matrix_UB_13 -0.0099380000
_diffrn_orient_matrix_UB_21 0.0208798000
_diffrn_orient_matrix_UB_22 -0.0405989000
_diffrn_orient_matrix_UB_23 -0.0201297000
_diffrn_orient_matrix_UB_31 0.0164847000
_diffrn_orient_matrix_UB_32 -0.0180227000
_diffrn_orient_matrix_UB_33 0.0539841000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3272
_reflns_number_total 4232
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.028
_refine_diff_density_min -0.778
_refine_diff_density_rms 0.140
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 253
_refine_ls_number_reflns 4232
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0589
_refine_ls_R_factor_gt 0.0394
_refine_ls_restrained_S_all 1.039
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0718
_refine_ls_wR_factor_ref 0.0813
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C8(H8), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C18(H18),
C19(H19), C20(H20)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
C1 C 0.7235(4) 0.3310(2) 0.5014(2) 0.0126(7) Uani 1 1 d . . . . .
C2 C 0.7546(4) 0.2427(3) 0.4888(2) 0.0171(8) Uani 1 1 d . . . . .
C3 C 0.6814(4) 0.1754(2) 0.5260(2) 0.0153(7) Uani 1 1 d . . . . .
C4 C 0.5743(4) 0.1970(3) 0.5768(2) 0.0167(8) Uani 1 1 d . . . . .
C5 C 0.5420(4) 0.2844(3) 0.5911(2) 0.0173(8) Uani 1 1 d . . . . .
C6 C 0.6157(4) 0.3508(2) 0.5522(2) 0.0149(7) Uani 1 1 d . . . . .
F1 F 0.8580(2) 0.22007(15) 0.43915(14) 0.0227(5) Uani 1 1 d . . . . .
F2 F 0.7137(2) 0.08981(14) 0.51374(15) 0.0227(5) Uani 1 1 d . . . . .
F3 F 0.5028(2) 0.13168(15) 0.61217(15) 0.0245(5) Uani 1 1 d . . . . .
F4 F 0.4385(2) 0.30546(15) 0.64030(14) 0.0235(5) Uani 1 1 d . . . . .
F5 F 0.5819(2) 0.43548(13) 0.56736(15) 0.0220(5) Uani 1 1 d . . . . .
I1 I 0.83589(2) 0.43248(2) 0.44793(2) 0.01982(9) Uani 1 1 d . . . . .
C7 C 0.5589(4) 0.3185(2) 0.2034(2) 0.0153(8) Uani 1 1 d . . . . .
C8 C 0.6590(4) 0.3441(3) 0.1468(2) 0.0165(8) Uani 1 1 d . . . . .
H8 H 0.7167 0.3020 0.1248 0.020 Uiso 1 1 calc R . . . .
C9 C 0.6713(4) 0.4336(3) 0.1238(3) 0.0178(8) Uani 1 1 d . . . . .
H9 H 0.7376 0.4515 0.0858 0.021 Uiso 1 1 calc R . . . .
C10 C 0.5856(4) 0.4969(3) 0.1569(2) 0.0182(8) Uani 1 1 d . . . . .
H10 H 0.5952 0.5565 0.1404 0.022 Uiso 1 1 calc R . . . .
C11 C 0.4859(4) 0.4725(3) 0.2142(2) 0.0167(8) Uani 1 1 d . . . . .
H11 H 0.4297 0.5153 0.2368 0.020 Uiso 1 1 calc R . . . .
C12 C 0.4714(3) 0.3837(2) 0.2371(2) 0.0135(7) Uani 1 1 d . . . . .
C13 C 0.3735(3) 0.3360(2) 0.2922(2) 0.0123(7) Uani 1 1 d . . . . .
C14 C 0.2660(4) 0.3610(3) 0.3404(2) 0.0173(8) Uani 1 1 d . . . . .
H14 H 0.2423 0.4206 0.3450 0.021 Uiso 1 1 calc R . . . .
C15 C 0.1919(4) 0.2928(3) 0.3830(3) 0.0202(8) Uani 1 1 d . . . . .
H15 H 0.1188 0.3092 0.4153 0.024 Uiso 1 1 calc R . . . .
C16 C 0.2243(4) 0.2039(3) 0.3782(2) 0.0195(8) Uani 1 1 d . . . . .
H16 H 0.1733 0.1616 0.4066 0.023 Uiso 1 1 calc R . . . .
C17 C 0.3362(4) 0.1766(2) 0.3295(2) 0.0155(8) Uani 1 1 d . . . . .
C18 C 0.3861(4) 0.0889(3) 0.3198(3) 0.0185(8) Uani 1 1 d . . . . .
H18 H 0.3437 0.0413 0.3467 0.022 Uiso 1 1 calc R . . . .
C19 C 0.4967(4) 0.0737(2) 0.2708(3) 0.0176(8) Uani 1 1 d . . . . .
H19 H 0.5275 0.0156 0.2651 0.021 Uiso 1 1 calc R . . . .
C20 C 0.5651(4) 0.1444(3) 0.2288(2) 0.0175(8) Uani 1 1 d . . . . .
H20 H 0.6401 0.1328 0.1966 0.021 Uiso 1 1 calc R . . . .
C21 C 0.5189(3) 0.2299(2) 0.2365(2) 0.0129(7) Uani 1 1 d . . . . .
C22 C 0.4056(3) 0.2442(2) 0.2878(2) 0.0144(7) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0146(17) 0.0138(19) 0.0081(14) 0.0028(14) 0.0006(12) -0.0014(15)
C2 0.0121(16) 0.026(2) 0.0133(16) -0.0002(16) 0.0032(13) 0.0043(17)
C3 0.0176(18) 0.0117(19) 0.0133(15) 0.0000(15) -0.0019(13) -0.0001(16)
C4 0.0158(17) 0.016(2) 0.0155(16) 0.0053(15) -0.0004(13) -0.0027(17)
C5 0.0151(17) 0.023(2) 0.0133(16) 0.0014(16) 0.0031(13) 0.0001(17)
C6 0.0151(17) 0.0128(19) 0.0148(16) -0.0001(15) 0.0005(13) 0.0017(16)
F1 0.0191(11) 0.0268(14) 0.0234(10) -0.0041(9) 0.0078(8) 0.0037(10)
F2 0.0270(12) 0.0118(12) 0.0257(10) -0.0032(9) 0.0005(9) 0.0028(10)
F3 0.0241(11) 0.0217(13) 0.0268(10) 0.0058(10) 0.0053(9) -0.0092(10)
F4 0.0187(11) 0.0300(14) 0.0257(10) -0.0004(10) 0.0130(8) 0.0007(10)
F5 0.0259(12) 0.0126(11) 0.0294(11) -0.0019(9) 0.0105(9) 0.0026(10)
I1 0.01868(13) 0.02161(15) 0.01856(13) 0.00330(10) 0.00381(9) -0.00660(11)
C7 0.0167(17) 0.017(2) 0.0099(15) -0.0023(14) -0.0004(12) -0.0030(16)
C8 0.0153(17) 0.019(2) 0.0151(16) 0.0001(16) 0.0031(13) 0.0007(16)
C9 0.0151(17) 0.025(2) 0.0137(16) 0.0047(16) 0.0046(13) -0.0053(17)
C10 0.0223(19) 0.013(2) 0.0170(17) 0.0047(15) 0.0008(14) 0.0003(17)
C11 0.0135(17) 0.018(2) 0.0174(16) -0.0006(15) 0.0014(13) -0.0001(16)
C12 0.0113(16) 0.018(2) 0.0097(15) -0.0003(15) -0.0006(12) 0.0011(16)
C13 0.0123(16) 0.0158(19) 0.0076(14) -0.0003(14) 0.0008(12) -0.0023(15)
C14 0.0130(17) 0.021(2) 0.0156(16) -0.0020(15) -0.0003(13) 0.0022(16)
C15 0.0148(17) 0.030(2) 0.0172(16) -0.0023(17) 0.0073(13) -0.0047(18)
C16 0.0169(18) 0.027(2) 0.0135(16) 0.0010(16) 0.0026(13) -0.0077(18)
C17 0.0132(17) 0.019(2) 0.0143(15) -0.0013(15) 0.0032(13) -0.0018(16)
C18 0.0200(19) 0.020(2) 0.0133(16) 0.0019(15) 0.0001(13) -0.0058(17)
C19 0.0200(18) 0.0113(19) 0.0185(17) -0.0014(15) -0.0004(14) 0.0015(16)
C20 0.0149(17) 0.022(2) 0.0156(16) -0.0021(16) 0.0043(13) 0.0015(17)
C21 0.0115(16) 0.016(2) 0.0093(15) 0.0001(14) -0.0001(12) -0.0006(15)
C22 0.0123(16) 0.017(2) 0.0128(15) -0.0002(15) 0.0011(13) 0.0009(15)
_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
C1 C2 1.378(5) . ?
C1 C6 1.383(5) . ?
C1 I1 2.079(3) . ?
C2 C3 1.382(5) . ?
C2 F1 1.347(4) . ?
C3 C4 1.383(5) . ?
C3 F2 1.341(4) . ?
C4 C5 1.373(5) . ?
C4 F3 1.339(4) . ?
C5 C6 1.384(5) . ?
C5 F4 1.338(4) . ?
C6 F5 1.340(4) . ?
C7 C8 1.391(5) . ?
C7 C12 1.426(5) . ?
C7 C21 1.476(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.388(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.391(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.390(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.380(5) . ?
C12 C13 1.489(5) . ?
C13 C14 1.378(5) . ?
C13 C22 1.419(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.429(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.378(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.428(5) . ?
C17 C18 1.418(5) . ?
C17 C22 1.391(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.379(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.422(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.371(5) . ?
C21 C22 1.418(4) . ?
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
C2 C1 C6 118.1(3) . . ?
C2 C1 I1 121.6(3) . . ?
C6 C1 I1 120.4(3) . . ?
C1 C2 C3 121.5(3) . . ?
F1 C2 C1 120.3(3) . . ?
F1 C2 C3 118.2(3) . . ?
C2 C3 C4 119.3(3) . . ?
F2 C3 C2 120.7(3) . . ?
F2 C3 C4 120.0(3) . . ?
C5 C4 C3 120.4(3) . . ?
F3 C4 C3 119.2(3) . . ?
F3 C4 C5 120.4(3) . . ?
C4 C5 C6 119.3(3) . . ?
F4 C5 C4 120.5(3) . . ?
F4 C5 C6 120.2(3) . . ?
C1 C6 C5 121.4(3) . . ?
F5 C6 C1 120.5(3) . . ?
F5 C6 C5 118.0(3) . . ?
C8 C7 C12 120.1(3) . . ?
C8 C7 C21 131.2(3) . . ?
C12 C7 C21 108.7(3) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 C7 118.9(3) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 H9 119.6 . . ?
C8 C9 C10 120.7(3) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10 119.5 . . ?
C10 C11 H11 120.5 . . ?
C12 C11 C10 119.0(3) . . ?
C12 C11 H11 120.5 . . ?
C7 C12 C13 107.4(3) . . ?
C11 C12 C7 120.2(3) . . ?
C11 C12 C13 132.3(3) . . ?
C14 C13 C12 135.2(3) . . ?
C14 C13 C22 118.5(3) . . ?
C22 C13 C12 106.3(3) . . ?
C13 C14 H14 120.9 . . ?
C13 C14 C15 118.2(3) . . ?
C15 C14 H14 120.9 . . ?
C14 C15 H15 118.7 . . ?
C16 C15 C14 122.6(3) . . ?
C16 C15 H15 118.7 . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.2(3) . . ?
C17 C16 H16 119.9 . . ?
C18 C17 C16 127.8(3) . . ?
C22 C17 C16 116.0(3) . . ?
C22 C17 C18 116.2(3) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.6(3) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 H19 119.1 . . ?
C18 C19 C20 121.8(3) . . ?
C20 C19 H19 119.1 . . ?
C19 C20 H20 120.5 . . ?
C21 C20 C19 119.0(3) . . ?
C21 C20 H20 120.5 . . ?
C20 C21 C7 135.5(3) . . ?
C20 C21 C22 118.3(3) . . ?
C22 C21 C7 106.2(3) . . ?
C17 C22 C13 124.5(3) . . ?
C17 C22 C21 124.1(3) . . ?
C21 C22 C13 111.4(3) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0.1(5) . . . . ?
C1 C2 C3 F2 -179.6(3) . . . . ?
C2 C1 C6 C5 0.9(5) . . . . ?
C2 C1 C6 F5 179.4(3) . . . . ?
C2 C3 C4 C5 -0.6(5) . . . . ?
C2 C3 C4 F3 179.6(3) . . . . ?
C3 C4 C5 C6 1.3(5) . . . . ?
C3 C4 C5 F4 -179.9(3) . . . . ?
C4 C5 C6 C1 -1.4(5) . . . . ?
C4 C5 C6 F5 -180.0(3) . . . . ?
C6 C1 C2 C3 -0.3(5) . . . . ?
C6 C1 C2 F1 179.6(3) . . . . ?
F1 C2 C3 C4 -179.7(3) . . . . ?
F1 C2 C3 F2 0.6(4) . . . . ?
F2 C3 C4 C5 179.1(3) . . . . ?
F2 C3 C4 F3 -0.7(4) . . . . ?
F3 C4 C5 C6 -178.9(3) . . . . ?
F3 C4 C5 F4 -0.2(5) . . . . ?
F4 C5 C6 C1 179.8(3) . . . . ?
F4 C5 C6 F5 1.2(4) . . . . ?
I1 C1 C2 C3 178.9(2) . . . . ?
I1 C1 C2 F1 -1.3(4) . . . . ?
I1 C1 C6 C5 -178.3(2) . . . . ?
I1 C1 C6 F5 0.2(4) . . . . ?
C7 C8 C9 C10 0.2(5) . . . . ?
C7 C12 C13 C14 -179.4(3) . . . . ?
C7 C12 C13 C22 -0.7(3) . . . . ?
C7 C21 C22 C13 -1.6(3) . . . . ?
C7 C21 C22 C17 179.2(3) . . . . ?
C8 C7 C12 C11 -0.2(4) . . . . ?
C8 C7 C12 C13 178.4(3) . . . . ?
C8 C7 C21 C20 2.9(6) . . . . ?
C8 C7 C21 C22 -177.4(3) . . . . ?
C8 C9 C10 C11 0.3(5) . . . . ?
C9 C10 C11 C12 -0.7(5) . . . . ?
C10 C11 C12 C7 0.7(4) . . . . ?
C10 C11 C12 C13 -177.6(3) . . . . ?
C11 C12 C13 C14 -1.0(6) . . . . ?
C11 C12 C13 C22 177.8(3) . . . . ?
C12 C7 C8 C9 -0.2(4) . . . . ?
C12 C7 C21 C20 -178.6(3) . . . . ?
C12 C7 C21 C22 1.1(3) . . . . ?
C12 C13 C14 C15 178.3(3) . . . . ?
C12 C13 C22 C17 -179.3(3) . . . . ?
C12 C13 C22 C21 1.4(3) . . . . ?
C13 C14 C15 C16 0.3(5) . . . . ?
C14 C13 C22 C17 -0.3(5) . . . . ?
C14 C13 C22 C21 -179.6(3) . . . . ?
C14 C15 C16 C17 0.2(5) . . . . ?
C15 C16 C17 C18 178.4(3) . . . . ?
C15 C16 C17 C22 -0.8(5) . . . . ?
C16 C17 C18 C19 -179.5(3) . . . . ?
C16 C17 C22 C13 0.9(5) . . . . ?
C16 C17 C22 C21 -179.9(3) . . . . ?
C17 C18 C19 C20 0.2(5) . . . . ?
C18 C17 C22 C13 -178.4(3) . . . . ?
C18 C17 C22 C21 0.8(5) . . . . ?
C18 C19 C20 C21 -0.5(5) . . . . ?
C19 C20 C21 C7 -179.4(3) . . . . ?
C19 C20 C21 C22 0.9(4) . . . . ?
C20 C21 C22 C13 178.2(3) . . . . ?
C20 C21 C22 C17 -1.1(5) . . . . ?
C21 C7 C8 C9 178.1(3) . . . . ?
C21 C7 C12 C11 -178.9(3) . . . . ?
C21 C7 C12 C13 -0.3(3) . . . . ?
C22 C13 C14 C15 -0.3(4) . . . . ?
C22 C17 C18 C19 -0.3(5) . . . . ?
_shelx_res_file
;
20161218b.res created by SHELXL-2014/7
TITL 20161218b_a.res in P2(1)/n
REM Old TITL 20161218b in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.085, Rweak 0.012, Alpha 0.029, Orientation as input
REM Formula found by SHELXT: C11 F5 I
CELL 0.71073 9.586009 15.035561 12.579817 90 105.2745 90
ZERR 4 0.000555 0.000688 0.000587 0 0.0053 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H F I
UNIT 88 40 20 4
L.S. 4
PLAN 5
BOND $H
MORE -1
CONF
fmap 2
acta 52
REM
REM
REM
WGHT 0.027800
FVAR 0.23274
C1 1 0.723491 0.330974 0.501360 11.00000 0.01456 0.01384 =
0.00810 0.00276 0.00056 -0.00142
C2 1 0.754625 0.242710 0.488803 11.00000 0.01210 0.02592 =
0.01332 -0.00016 0.00316 0.00429
C3 1 0.681391 0.175363 0.526011 11.00000 0.01759 0.01171 =
0.01326 0.00001 -0.00189 -0.00012
C4 1 0.574283 0.197023 0.576795 11.00000 0.01583 0.01624 =
0.01546 0.00530 -0.00035 -0.00268
C5 1 0.541995 0.284440 0.591087 11.00000 0.01506 0.02324 =
0.01335 0.00144 0.00311 0.00013
C6 1 0.615696 0.350764 0.552212 11.00000 0.01507 0.01278 =
0.01479 -0.00014 0.00051 0.00172
F1 3 0.858041 0.220069 0.439150 11.00000 0.01912 0.02675 =
0.02340 -0.00408 0.00780 0.00368
F2 3 0.713664 0.089809 0.513739 11.00000 0.02699 0.01179 =
0.02569 -0.00321 0.00052 0.00280
F3 3 0.502819 0.131675 0.612172 11.00000 0.02409 0.02175 =
0.02676 0.00581 0.00527 -0.00921
F4 3 0.438513 0.305462 0.640304 11.00000 0.01874 0.03003 =
0.02574 -0.00036 0.01301 0.00066
F5 3 0.581924 0.435475 0.567362 11.00000 0.02588 0.01258 =
0.02942 -0.00185 0.01055 0.00261
I1 4 0.835888 0.432483 0.447935 11.00000 0.01868 0.02161 =
0.01856 0.00330 0.00381 -0.00660
C7 1 0.558853 0.318517 0.203431 11.00000 0.01668 0.01716 =
0.00991 -0.00232 -0.00042 -0.00300
C8 1 0.658970 0.344109 0.146847 11.00000 0.01528 0.01864 =
0.01510 0.00007 0.00310 0.00072
AFIX 43
H8 2 0.716655 0.301961 0.124820 11.00000 -1.20000
AFIX 0
C9 1 0.671308 0.433615 0.123823 11.00000 0.01511 0.02517 =
0.01366 0.00467 0.00459 -0.00532
AFIX 43
H9 2 0.737642 0.451464 0.085831 11.00000 -1.20000
AFIX 0
C10 1 0.585592 0.496898 0.156930 11.00000 0.02226 0.01290 =
0.01702 0.00471 0.00082 0.00026
AFIX 43
H10 2 0.595168 0.556514 0.140449 11.00000 -1.20000
AFIX 0
C11 1 0.485851 0.472496 0.214245 11.00000 0.01352 0.01764 =
0.01741 -0.00055 0.00142 -0.00007
AFIX 43
H11 2 0.429748 0.515321 0.236814 11.00000 -1.20000
AFIX 0
C12 1 0.471363 0.383733 0.237140 11.00000 0.01126 0.01774 =
0.00973 -0.00031 -0.00060 0.00106
C13 1 0.373477 0.336005 0.292158 11.00000 0.01230 0.01583 =
0.00763 -0.00032 0.00078 -0.00226
C14 1 0.265981 0.360981 0.340381 11.00000 0.01300 0.02093 =
0.01561 -0.00196 -0.00033 0.00222
AFIX 43
H14 2 0.242317 0.420579 0.345048 11.00000 -1.20000
AFIX 0
C15 1 0.191858 0.292841 0.383019 11.00000 0.01483 0.03016 =
0.01724 -0.00231 0.00728 -0.00472
AFIX 43
H15 2 0.118844 0.309170 0.415306 11.00000 -1.20000
AFIX 0
C16 1 0.224329 0.203924 0.378164 11.00000 0.01689 0.02732 =
0.01350 0.00101 0.00264 -0.00770
AFIX 43
H16 2 0.173285 0.161614 0.406647 11.00000 -1.20000
AFIX 0
C17 1 0.336179 0.176565 0.329500 11.00000 0.01321 0.01877 =
0.01425 -0.00132 0.00317 -0.00184
C18 1 0.386052 0.088915 0.319808 11.00000 0.01997 0.01966 =
0.01332 0.00192 0.00008 -0.00583
AFIX 43
H18 2 0.343743 0.041261 0.346728 11.00000 -1.20000
AFIX 0
C19 1 0.496736 0.073693 0.270821 11.00000 0.02002 0.01133 =
0.01848 -0.00141 -0.00043 0.00152
AFIX 43
H19 2 0.527458 0.015639 0.265121 11.00000 -1.20000
AFIX 0
C20 1 0.565119 0.144395 0.228805 11.00000 0.01488 0.02220 =
0.01557 -0.00214 0.00434 0.00154
AFIX 43
H20 2 0.640110 0.132825 0.196581 11.00000 -1.20000
AFIX 0
C21 1 0.518901 0.229895 0.236483 11.00000 0.01149 0.01621 =
0.00935 0.00015 -0.00011 -0.00058
C22 1 0.405553 0.244150 0.287756 11.00000 0.01226 0.01685 =
0.01280 -0.00023 0.00106 0.00090
HKLF 4
REM 20161218b_a.res in P2(1)/n
REM R1 = 0.0394 for 3272 Fo > 4sig(Fo) and 0.0589 for all 4232 data
REM 253 parameters refined using 0 restraints
END
WGHT 0.0278 0.0000
REM Highest difference peak 1.028, deepest hole -0.778, 1-sigma level 0.140
Q1 1 0.5124 0.5704 0.3445 11.00000 0.05 1.03
Q2 1 0.6726 0.2035 0.0577 11.00000 0.05 0.79
Q3 1 0.8587 0.4607 0.5369 11.00000 0.05 0.63
Q4 1 0.7977 0.4073 0.3770 11.00000 0.05 0.62
Q5 1 0.9025 0.3966 0.5118 11.00000 0.05 0.60
;
_shelx_res_checksum 69835
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.129
_oxdiff_exptl_absorpt_empirical_full_min 0.659
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_20161209c
_database_code_depnum_ccdc_archive 'CCDC 1547627'
_audit_update_record
;
2017-07-20 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_audit_creation_date 2016-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common ?
_chemical_name_systematic 14DIPB-FA
_chemical_formula_moiety 'C6 F4 I2, C16 H10'
_chemical_formula_sum 'C22 H10 F4 I2'
_chemical_formula_weight 604.10
_chemical_melting_point ?
_chemical_oxdiff_formula c1h1f1i1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'
_cell_length_a 8.3808(6)
_cell_length_b 18.0644(10)
_cell_length_c 12.8815(10)
_cell_angle_alpha 90.00
_cell_angle_beta 105.561(9)
_cell_angle_gamma 90.00
_cell_volume 1878.7(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 3700
_cell_measurement_temperature 100.01(10)
_cell_measurement_theta_max 28.8300
_cell_measurement_theta_min 3.4630
_exptl_absorpt_coefficient_mu 3.391
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.81137
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 2.136
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1136
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_special_details
;
?
;
_diffrn_reflns_av_R_equivalents 0.0438
_diffrn_reflns_av_unetI/netI 0.0587
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 8584
_diffrn_reflns_theta_full 25.35
_diffrn_reflns_theta_max 25.35
_diffrn_reflns_theta_min 3.38
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.8487
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -43.00 37.00 1.00 1.00 -- 12.76 -37.00 -30.00 80
2 \w -20.00 61.00 1.00 1.00 -- 12.76 77.00 150.00 81
3 \w -29.00 14.00 1.00 1.00 -- 12.76 -37.00 30.00 43
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0846377000
_diffrn_orient_matrix_UB_12 0.0070002000
_diffrn_orient_matrix_UB_13 0.0256818000
_diffrn_orient_matrix_UB_21 -0.0158903000
_diffrn_orient_matrix_UB_22 0.0386277000
_diffrn_orient_matrix_UB_23 -0.0032677000
_diffrn_orient_matrix_UB_31 -0.0172434000
_diffrn_orient_matrix_UB_32 -0.0010757000
_diffrn_orient_matrix_UB_33 0.0509687000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_reflns_number_gt 2898
_reflns_number_total 3419
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_threshold_expression >2sigma(I)
_computing_cell_refinement 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max 0.637
_refine_diff_density_min -0.533
_refine_diff_density_rms 0.137
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 253
_refine_ls_number_reflns 3419
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0406
_refine_ls_R_factor_gt 0.0316
_refine_ls_restrained_S_all 1.028
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0098P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0570
_refine_ls_wR_factor_ref 0.0617
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C26(H26), C18(H18), C25(H25), C28(H28), C27(H27), C16(H16), C20(H20),
C19(H19), C15(H15), C14(H14)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
I8 I 0.15906(4) 0.720205(14) 0.26384(2) 0.01845(10) Uani 1 d . . .
I7 I 0.58163(4) 1.053514(15) 0.27178(3) 0.02360(10) Uani 1 d . . .
F9 F 0.3901(3) 0.81478(13) 0.45519(17) 0.0233(6) Uani 1 d . . .
F12 F 0.1779(3) 0.83480(13) 0.07682(18) 0.0256(6) Uani 1 d . . .
F10 F 0.5607(3) 0.93896(12) 0.45803(18) 0.0236(6) Uani 1 d . . .
F11 F 0.3419(3) 0.96142(13) 0.08110(19) 0.0275(7) Uani 1 d . . .
C4 C 0.2820(5) 0.8207(2) 0.2660(3) 0.0134(10) Uani 1 d . . .
C26 C 1.1524(6) 0.4278(2) 0.8130(3) 0.0197(10) Uani 1 d . . .
H26 H 1.2247 0.3921 0.8511 0.024 Uiso 1 calc . . R
C24 C 1.0045(5) 0.5404(2) 0.8103(3) 0.0122(9) Uani 1 d . . .
C18 C 0.6139(6) 0.7195(2) 0.6506(3) 0.0164(10) Uani 1 d . . .
H18 H 0.5468 0.7611 0.6450 0.020 Uiso 1 calc . . R
C25 C 1.0865(6) 0.4201(2) 0.7024(3) 0.0189(10) Uani 1 d . . .
H25 H 1.1172 0.3798 0.6671 0.023 Uiso 1 calc . . R
C5 C 0.2706(5) 0.8600(2) 0.1725(3) 0.0147(10) Uani 1 d . . .
C28 C 0.9750(6) 0.4720(2) 0.6434(3) 0.0169(10) Uani 1 d . . .
H28 H 0.9294 0.4661 0.5697 0.020 Uiso 1 calc . . R
C27 C 1.1112(6) 0.4884(2) 0.8673(3) 0.0182(10) Uani 1 d . . .
H27 H 1.1555 0.4935 0.9413 0.022 Uiso 1 calc . . R
C2 C 0.4652(6) 0.9145(2) 0.3630(3) 0.0172(10) Uani 1 d . . .
C17 C 0.7244(5) 0.7003(2) 0.7515(3) 0.0134(10) Uani 1 d . . .
C22 C 0.8200(6) 0.6371(2) 0.7524(3) 0.0144(10) Uani 1 d . . .
C23 C 0.9334(5) 0.5325(2) 0.6971(3) 0.0140(10) Uani 1 d . . .
C1 C 0.4535(6) 0.9545(2) 0.2698(3) 0.0164(10) Uani 1 d . . .
C3 C 0.3778(6) 0.8496(2) 0.3617(3) 0.0151(10) Uani 1 d . . .
C16 C 0.7457(6) 0.7360(2) 0.8516(3) 0.0169(10) Uani 1 d . . .
H16 H 0.6836 0.7779 0.8563 0.020 Uiso 1 calc . . R
C21 C 0.8161(5) 0.5939(2) 0.6596(3) 0.0141(10) Uani 1 d . . .
C6 C 0.3572(6) 0.9261(2) 0.1752(3) 0.0185(10) Uani 1 d . . .
C13 C 0.9334(5) 0.6090(2) 0.8448(3) 0.0140(10) Uani 1 d . . .
C20 C 0.7078(6) 0.6133(2) 0.5639(3) 0.0181(10) Uani 1 d . . .
H20 H 0.7009 0.5857 0.5019 0.022 Uiso 1 calc . . R
C19 C 0.6061(6) 0.6764(2) 0.5610(3) 0.0193(11) Uani 1 d . . .
H19 H 0.5313 0.6893 0.4961 0.023 Uiso 1 calc . . R
C15 C 0.8570(6) 0.7095(2) 0.9421(3) 0.0188(11) Uani 1 d . . .
H15 H 0.8701 0.7347 1.0068 0.023 Uiso 1 calc . . R
C14 C 0.9533(6) 0.6449(2) 0.9406(3) 0.0186(10) Uani 1 d . . .
H14 H 1.0277 0.6276 1.0030 0.022 Uiso 1 calc . . R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I8 0.01836(19) 0.01202(16) 0.02712(17) -0.00071(12) 0.00980(14) -0.00057(12)
I7 0.0167(2) 0.01391(16) 0.0426(2) -0.00196(13) 0.01221(16) -0.00118(13)
F9 0.0324(18) 0.0218(14) 0.0153(12) 0.0033(11) 0.0054(13) 0.0036(12)
F12 0.0259(17) 0.0295(15) 0.0179(13) 0.0014(11) -0.0002(13) -0.0082(12)
F10 0.0212(17) 0.0228(14) 0.0220(13) -0.0074(11) -0.0027(13) -0.0010(12)
F11 0.0365(19) 0.0227(14) 0.0226(13) 0.0124(12) 0.0070(14) 0.0003(13)
C4 0.013(3) 0.009(2) 0.021(2) -0.0001(18) 0.008(2) 0.0000(18)
C26 0.013(3) 0.015(2) 0.032(3) 0.006(2) 0.008(2) 0.0013(19)
C24 0.014(3) 0.007(2) 0.016(2) 0.0028(17) 0.006(2) -0.0028(18)
C18 0.018(3) 0.009(2) 0.025(2) 0.0028(19) 0.011(2) 0.0001(19)
C25 0.018(3) 0.013(2) 0.028(2) -0.002(2) 0.010(2) -0.004(2)
C5 0.011(3) 0.016(2) 0.016(2) -0.0027(18) 0.002(2) 0.0003(19)
C28 0.019(3) 0.017(2) 0.016(2) -0.0006(19) 0.007(2) -0.001(2)
C27 0.015(3) 0.018(2) 0.020(2) 0.008(2) 0.003(2) -0.007(2)
C2 0.015(3) 0.018(2) 0.019(2) -0.0029(19) 0.004(2) 0.003(2)
C17 0.015(3) 0.012(2) 0.017(2) 0.0032(18) 0.011(2) -0.0034(19)
C22 0.019(3) 0.011(2) 0.016(2) 0.0035(18) 0.008(2) -0.0074(19)
C23 0.014(3) 0.012(2) 0.019(2) 0.0008(18) 0.009(2) -0.0041(18)
C1 0.013(3) 0.011(2) 0.027(2) -0.0036(19) 0.009(2) 0.0031(19)
C3 0.017(3) 0.014(2) 0.018(2) 0.0065(18) 0.011(2) 0.0088(19)
C16 0.017(3) 0.014(2) 0.022(2) -0.0008(19) 0.009(2) -0.0012(19)
C21 0.011(3) 0.014(2) 0.019(2) 0.0006(18) 0.008(2) -0.0016(19)
C6 0.018(3) 0.018(2) 0.018(2) 0.0066(19) 0.004(2) 0.003(2)
C13 0.013(3) 0.013(2) 0.019(2) -0.0022(18) 0.009(2) -0.0060(18)
C20 0.023(3) 0.019(2) 0.012(2) 0.0020(19) 0.005(2) 0.001(2)
C19 0.021(3) 0.020(2) 0.017(2) 0.010(2) 0.006(2) 0.000(2)
C15 0.023(3) 0.020(2) 0.018(2) -0.0043(19) 0.013(2) -0.006(2)
C14 0.017(3) 0.022(2) 0.017(2) 0.0019(19) 0.006(2) -0.008(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
I8 C4 2.083(4) . ?
I7 C1 2.083(4) . ?
F9 C3 1.338(4) . ?
F12 C5 1.348(5) . ?
F10 C2 1.344(5) . ?
F11 C6 1.345(4) . ?
C4 C5 1.380(5) . ?
C4 C3 1.380(6) . ?
C26 H26 0.9300 . ?
C26 C25 1.391(6) . ?
C26 C27 1.392(6) . ?
C24 C27 1.367(6) . ?
C24 C23 1.426(6) . ?
C24 C13 1.493(5) . ?
C18 H18 0.9300 . ?
C18 C17 1.422(6) . ?
C18 C19 1.379(5) . ?
C25 H25 0.9300 . ?
C25 C28 1.396(6) . ?
C5 C6 1.392(6) . ?
C28 H28 0.9300 . ?
C28 C23 1.386(5) . ?
C27 H27 0.9300 . ?
C2 C1 1.382(6) . ?
C2 C3 1.381(6) . ?
C17 C22 1.393(6) . ?
C17 C16 1.410(5) . ?
C22 C21 1.422(5) . ?
C22 C13 1.404(6) . ?
C23 C21 1.475(6) . ?
C1 C6 1.369(6) . ?
C16 H16 0.9300 . ?
C16 C15 1.369(6) . ?
C21 C20 1.367(6) . ?
C13 C14 1.363(5) . ?
C20 H20 0.9300 . ?
C20 C19 1.417(6) . ?
C19 H19 0.9300 . ?
C15 H15 0.9300 . ?
C15 C14 1.423(6) . ?
C14 H14 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 C4 I8 121.3(3) . . ?
C3 C4 I8 120.6(3) . . ?
C3 C4 C5 118.2(4) . . ?
C25 C26 H26 119.7 . . ?
C25 C26 C27 120.7(4) . . ?
C27 C26 H26 119.7 . . ?
C27 C24 C23 120.9(4) . . ?
C27 C24 C13 131.7(4) . . ?
C23 C24 C13 107.3(4) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C19 C18 C17 120.1(4) . . ?
C26 C25 H25 119.5 . . ?
C26 C25 C28 121.0(4) . . ?
C28 C25 H25 119.5 . . ?
F12 C5 C4 120.8(4) . . ?
F12 C5 C6 118.7(3) . . ?
C4 C5 C6 120.5(4) . . ?
C25 C28 H28 120.7 . . ?
C23 C28 C25 118.6(4) . . ?
C23 C28 H28 120.7 . . ?
C26 C27 H27 120.5 . . ?
C24 C27 C26 119.0(4) . . ?
C24 C27 H27 120.5 . . ?
F10 C2 C1 120.4(4) . . ?
F10 C2 C3 118.3(4) . . ?
C3 C2 C1 121.3(4) . . ?
C22 C17 C18 116.1(4) . . ?
C22 C17 C16 115.8(4) . . ?
C16 C17 C18 128.1(4) . . ?
C17 C22 C21 124.0(4) . . ?
C17 C22 C13 124.1(4) . . ?
C13 C22 C21 111.8(4) . . ?
C24 C23 C21 108.5(3) . . ?
C28 C23 C24 119.8(4) . . ?
C28 C23 C21 131.6(4) . . ?
C2 C1 I7 121.5(3) . . ?
C6 C1 I7 120.8(3) . . ?
C6 C1 C2 117.7(4) . . ?
F9 C3 C4 120.8(4) . . ?
F9 C3 C2 118.4(4) . . ?
C4 C3 C2 120.8(4) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 C17 120.6(4) . . ?
C15 C16 H16 119.7 . . ?
C22 C21 C23 106.0(4) . . ?
C20 C21 C22 118.5(4) . . ?
C20 C21 C23 135.4(4) . . ?
F11 C6 C5 117.5(4) . . ?
F11 C6 C1 121.0(4) . . ?
C1 C6 C5 121.5(4) . . ?
C22 C13 C24 106.3(3) . . ?
C14 C13 C24 134.6(4) . . ?
C14 C13 C22 119.0(4) . . ?
C21 C20 H20 120.6 . . ?
C21 C20 C19 118.7(4) . . ?
C19 C20 H20 120.6 . . ?
C18 C19 C20 122.5(4) . . ?
C18 C19 H19 118.7 . . ?
C20 C19 H19 118.7 . . ?
C16 C15 H15 118.8 . . ?
C16 C15 C14 122.3(4) . . ?
C14 C15 H15 118.8 . . ?
C13 C14 C15 118.1(4) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
I8 C4 C5 F12 0.6(5) . . . . ?
I8 C4 C5 C6 -178.2(3) . . . . ?
I8 C4 C3 F9 -1.8(5) . . . . ?
I8 C4 C3 C2 177.2(3) . . . . ?
I7 C1 C6 F11 -0.5(6) . . . . ?
I7 C1 C6 C5 -179.9(3) . . . . ?
F12 C5 C6 F11 0.6(6) . . . . ?
F12 C5 C6 C1 -180.0(4) . . . . ?
F10 C2 C1 I7 0.0(5) . . . . ?
F10 C2 C1 C6 178.6(4) . . . . ?
F10 C2 C3 F9 1.1(6) . . . . ?
F10 C2 C3 C4 -177.9(4) . . . . ?
C4 C5 C6 F11 179.5(4) . . . . ?
C4 C5 C6 C1 -1.1(7) . . . . ?
C26 C25 C28 C23 1.3(6) . . . . ?
C24 C23 C21 C22 -0.2(5) . . . . ?
C24 C23 C21 C20 -176.0(5) . . . . ?
C24 C13 C14 C15 -178.0(4) . . . . ?
C18 C17 C22 C21 2.1(6) . . . . ?
C18 C17 C22 C13 -178.7(4) . . . . ?
C18 C17 C16 C15 179.1(4) . . . . ?
C25 C26 C27 C24 0.1(6) . . . . ?
C25 C28 C23 C24 -0.1(6) . . . . ?
C25 C28 C23 C21 -176.8(4) . . . . ?
C5 C4 C3 F9 178.3(4) . . . . ?
C5 C4 C3 C2 -2.6(6) . . . . ?
C28 C23 C21 C22 176.9(4) . . . . ?
C28 C23 C21 C20 1.1(8) . . . . ?
C27 C26 C25 C28 -1.4(6) . . . . ?
C27 C24 C23 C28 -1.2(6) . . . . ?
C27 C24 C23 C21 176.3(4) . . . . ?
C27 C24 C13 C22 -175.0(4) . . . . ?
C27 C24 C13 C14 3.4(8) . . . . ?
C2 C1 C6 F11 -179.1(4) . . . . ?
C2 C1 C6 C5 1.5(6) . . . . ?
C17 C18 C19 C20 -1.4(6) . . . . ?
C17 C22 C21 C23 -179.3(4) . . . . ?
C17 C22 C21 C20 -2.6(6) . . . . ?
C17 C22 C13 C24 178.6(4) . . . . ?
C17 C22 C13 C14 -0.1(6) . . . . ?
C17 C16 C15 C14 -1.2(6) . . . . ?
C22 C17 C16 C15 1.3(6) . . . . ?
C22 C21 C20 C19 1.0(6) . . . . ?
C22 C13 C14 C15 0.2(6) . . . . ?
C23 C24 C27 C26 1.2(6) . . . . ?
C23 C24 C13 C22 2.0(4) . . . . ?
C23 C24 C13 C14 -179.7(4) . . . . ?
C23 C21 C20 C19 176.4(4) . . . . ?
C1 C2 C3 F9 -177.8(4) . . . . ?
C1 C2 C3 C4 3.2(6) . . . . ?
C3 C4 C5 F12 -179.5(4) . . . . ?
C3 C4 C5 C6 1.6(6) . . . . ?
C3 C2 C1 I7 178.9(3) . . . . ?
C3 C2 C1 C6 -2.5(6) . . . . ?
C16 C17 C22 C21 -179.8(4) . . . . ?
C16 C17 C22 C13 -0.7(6) . . . . ?
C16 C15 C14 C13 0.4(6) . . . . ?
C21 C22 C13 C24 -2.1(5) . . . . ?
C21 C22 C13 C14 179.2(4) . . . . ?
C21 C20 C19 C18 0.9(6) . . . . ?
C13 C24 C27 C26 177.8(4) . . . . ?
C13 C24 C23 C28 -178.6(4) . . . . ?
C13 C24 C23 C21 -1.1(4) . . . . ?
C13 C22 C21 C23 1.5(5) . . . . ?
C13 C22 C21 C20 178.1(4) . . . . ?
C19 C18 C17 C22 -0.1(6) . . . . ?
C19 C18 C17 C16 -177.9(4) . . . . ?
_iucr_refine_instructions_details
;
TITL 20161209c_a.res in P2(1)/c
REM Old TITL 20161209c in P21/c #14
REM SHELXT solution in P2(1)/c
REM R1 0.113, Rweak 0.008, Alpha 0.050, Orientation as input
REM Formula found by SHELXT: C22 F4 I2
CELL 0.71073 8.3808 18.0644 12.8815 90 105.561 90
ZERR 4 0.0006 0.001 0.001 0 0.009 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H F I
UNIT 88 40 16 8
L.S. 10
PLAN 5
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
SHEL 999 0.83
REM
REM
REM
WGHT 0.009800
FVAR 0.21986
I8 4 0.159057 0.720205 0.263836 11.00000 0.01836 0.01202 =
0.02712 -0.00071 0.00980 -0.00057
I7 4 0.581629 1.053514 0.271783 11.00000 0.01672 0.01391 =
0.04262 -0.00196 0.01221 -0.00118
F9 3 0.390127 0.814783 0.455185 11.00000 0.03237 0.02176 =
0.01528 0.00325 0.00537 0.00358
F12 3 0.177923 0.834804 0.076821 11.00000 0.02587 0.02954 =
0.01792 0.00137 -0.00023 -0.00824
F10 3 0.560656 0.938958 0.458035 11.00000 0.02121 0.02283 =
0.02197 -0.00744 -0.00265 -0.00105
F11 3 0.341886 0.961423 0.081101 11.00000 0.03650 0.02269 =
0.02264 0.01235 0.00698 0.00030
C4 1 0.282015 0.820673 0.266043 11.00000 0.01261 0.00877 =
0.02115 -0.00006 0.00847 0.00004
C26 1 1.152362 0.427785 0.813029 11.00000 0.01335 0.01502 =
0.03218 0.00626 0.00849 0.00133
AFIX 43
H26 2 1.224665 0.392064 0.851132 11.00000 -1.20000
AFIX 0
C24 1 1.004464 0.540434 0.810275 11.00000 0.01444 0.00708 =
0.01631 0.00275 0.00629 -0.00282
C18 1 0.613904 0.719466 0.650557 11.00000 0.01837 0.00921 =
0.02491 0.00280 0.01128 0.00005
AFIX 43
H18 2 0.546789 0.761077 0.644982 11.00000 -1.20000
AFIX 0
C25 1 1.086481 0.420103 0.702370 11.00000 0.01836 0.01279 =
0.02756 -0.00222 0.00977 -0.00419
AFIX 43
H25 2 1.117175 0.379805 0.667123 11.00000 -1.20000
AFIX 0
C5 1 0.270611 0.860043 0.172546 11.00000 0.01100 0.01632 =
0.01553 -0.00272 0.00160 0.00032
C28 1 0.974962 0.471996 0.643443 11.00000 0.01919 0.01659 =
0.01613 -0.00061 0.00672 -0.00055
AFIX 43
H28 2 0.929448 0.466129 0.569690 11.00000 -1.20000
AFIX 0
C27 1 1.111152 0.488419 0.867333 11.00000 0.01544 0.01790 =
0.02019 0.00827 0.00266 -0.00740
AFIX 43
H27 2 1.155524 0.493477 0.941324 11.00000 -1.20000
AFIX 0
C2 1 0.465162 0.914532 0.363026 11.00000 0.01469 0.01769 =
0.01879 -0.00294 0.00357 0.00290
C17 1 0.724415 0.700312 0.751468 11.00000 0.01542 0.01180 =
0.01684 0.00323 0.01078 -0.00336
C22 1 0.820018 0.637128 0.752444 11.00000 0.01855 0.01056 =
0.01595 0.00350 0.00772 -0.00743
C23 1 0.933442 0.532465 0.697125 11.00000 0.01384 0.01197 =
0.01879 0.00078 0.00877 -0.00413
C1 1 0.453489 0.954523 0.269819 11.00000 0.01323 0.01068 =
0.02736 -0.00358 0.00915 0.00312
C3 1 0.377756 0.849563 0.361665 11.00000 0.01701 0.01386 =
0.01793 0.00647 0.01054 0.00876
C16 1 0.745734 0.735992 0.851623 11.00000 0.01662 0.01402 =
0.02212 -0.00082 0.00880 -0.00121
AFIX 43
H16 2 0.683606 0.777917 0.856253 11.00000 -1.20000
AFIX 0
C21 1 0.816128 0.593862 0.659619 11.00000 0.01145 0.01414 =
0.01869 0.00057 0.00763 -0.00158
C6 1 0.357228 0.926060 0.175164 11.00000 0.01825 0.01845 =
0.01846 0.00659 0.00426 0.00296
C13 1 0.933353 0.608969 0.844847 11.00000 0.01341 0.01274 =
0.01868 -0.00218 0.00908 -0.00599
C20 1 0.707772 0.613333 0.563910 11.00000 0.02328 0.01882 =
0.01214 0.00204 0.00455 0.00101
AFIX 43
H20 2 0.700872 0.585721 0.501925 11.00000 -1.20000
AFIX 0
C19 1 0.606129 0.676416 0.560952 11.00000 0.02140 0.02022 =
0.01659 0.01022 0.00554 -0.00004
AFIX 43
H19 2 0.531283 0.689274 0.496057 11.00000 -1.20000
AFIX 0
C15 1 0.856996 0.709512 0.942098 11.00000 0.02287 0.02002 =
0.01779 -0.00428 0.01275 -0.00622
AFIX 43
H15 2 0.870094 0.734657 1.006847 11.00000 -1.20000
AFIX 0
C14 1 0.953320 0.644861 0.940556 11.00000 0.01722 0.02203 =
0.01730 0.00186 0.00569 -0.00768
AFIX 43
H14 2 1.027747 0.627595 1.003044 11.00000 -1.20000
HKLF 4
REM 20161209c_a.res in P2(1)/c
REM R1 = 0.0316 for 2898 Fo > 4sig(Fo) and 0.0406 for all 3419 data
REM 253 parameters refined using 0 restraints
END
WGHT 0.0098 0.0000
REM Highest difference peak 0.637, deepest hole -0.533, 1-sigma level 0.137
Q1 1 0.7059 1.0570 0.3389 11.00000 0.05 0.64
Q2 1 0.7974 0.7679 0.6857 11.00000 0.05 0.56
Q3 1 0.0426 0.7059 0.2067 11.00000 0.05 0.55
Q4 1 0.5268 1.0721 0.3613 11.00000 0.05 0.55
Q5 1 1.1023 0.4627 0.6874 11.00000 0.05 0.53
REM The information below was added by Olex2.
REM
REM R1 = 0.0316 for 2898 Fo > 4sig(Fo) and 0.0406 for all 10363 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.64, deepest hole -0.53
REM Mean Shift 0, Max Shift -0.003.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0406
REM R1_gt = 0.0316
REM wR_ref = 0.0617
REM GOOF = 1.028
REM Shift_max = -0.003
REM Shift_mean = 0
REM Reflections_all = 10363
REM Reflections_gt = 2898
REM Parameters = n/a
REM Hole = -0.53
REM Peak = 0.64
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.276
_oxdiff_exptl_absorpt_empirical_full_min 0.830
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_20161202a
_database_code_depnum_ccdc_archive 'CCDC 1547633'
_audit_update_record
;
2017-05-03 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_audit_creation_date 2016-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '2(Br2 C6 F4), 2(C16 H10)'
_chemical_formula_sum 'C44 H20 Br4 F8'
_chemical_formula_weight 1020.24
_chemical_melting_point ?
_chemical_oxdiff_formula c1h1f1Br1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 7.4059(8)
_cell_length_b 8.0966(9)
_cell_length_c 29.6317(13)
_cell_angle_alpha 88.510(6)
_cell_angle_beta 88.482(6)
_cell_angle_gamma 88.186(9)
_cell_volume 1774.7(3)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6386
_cell_measurement_temperature 100.01(10)
_cell_measurement_theta_max 29.1840
_cell_measurement_theta_min 3.9320
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 4.613
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.19190
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.909
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 992
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.3
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents ?
_diffrn_reflns_av_unetI/netI 0.1098
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 41
_diffrn_reflns_limit_l_min -40
_diffrn_reflns_number 8538
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 29.851
_diffrn_reflns_theta_min 3.296
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w 10.00 57.00 1.00 10.00 -- 12.76 37.00 120.00 47
2 \w -16.00 85.00 1.00 10.00 -- 12.76 77.00 150.00 101
3 \w -20.00 54.00 1.00 10.00 -- 12.76 -99.00 0.00 74
4 \w 15.00 54.00 1.00 10.00 -- 12.76 -99.00 -90.00 39
5 \w -54.00 32.00 1.00 10.00 -- 12.76 -37.00-120.00 86
6 \w -59.00 -28.00 1.00 10.00 -- 12.76 -37.00-150.00 31
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0778604000
_diffrn_orient_matrix_UB_12 -0.0516587000
_diffrn_orient_matrix_UB_13 -0.0037537000
_diffrn_orient_matrix_UB_21 -0.0328330000
_diffrn_orient_matrix_UB_22 -0.0576915000
_diffrn_orient_matrix_UB_23 0.0164023000
_diffrn_orient_matrix_UB_31 -0.0452921000
_diffrn_orient_matrix_UB_32 -0.0410590000
_diffrn_orient_matrix_UB_33 -0.0170473000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6311
_reflns_number_total 8538
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_special_details
;
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 2.973
_refine_diff_density_min -2.507
_refine_diff_density_rms 0.382
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.099
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 508
_refine_ls_number_reflns 8538
_refine_ls_number_restraints 312
_refine_ls_R_factor_all 0.1376
_refine_ls_R_factor_gt 0.1096
_refine_ls_restrained_S_all 1.084
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+81.3779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3018
_refine_ls_wR_factor_ref 0.3162
_refine_special_details
;
Refined as a 4-component twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.61(14) 0.13(8) 0.13(8) 0.13(8)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq,
Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim
Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F5) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22),
C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C36(H36),
C37(H37), C38(H38), C42(H42), C43(H43), C44(H44)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
Br1 Br -0.14511(19) 0.3472(2) 0.72234(4) 0.0212(3) Uani 1 1 d . . . . .
Br2 Br 0.00153(19) -0.01147(18) 0.67459(5) 0.0217(3) Uani 1 1 d . . . . .
C1 C -0.0637(17) 0.3368(17) 0.6621(4) 0.014(3) Uani 1 1 d . U . . .
C2 C 0.0059(18) 0.1928(17) 0.6434(4) 0.013(2) Uani 1 1 d . U . . .
C3 C 0.0779(18) 0.1959(18) 0.5996(5) 0.017(3) Uani 1 1 d . U . . .
C4 C 0.0747(18) 0.343(2) 0.5742(5) 0.019(3) Uani 1 1 d . U . . .
C5 C 0.000(2) 0.4864(19) 0.5924(5) 0.020(3) Uani 1 1 d . U . . .
C6 C -0.0648(19) 0.4827(18) 0.6367(5) 0.017(3) Uani 1 1 d . U . . .
F1 F 0.1456(12) 0.0598(12) 0.5809(3) 0.027(2) Uani 1 1 d . U . . .
F2 F 0.1423(12) 0.3443(13) 0.5324(3) 0.029(2) Uani 1 1 d . U . . .
F3 F -0.0041(13) 0.6261(13) 0.5678(3) 0.032(2) Uani 1 1 d . U . . .
F4 F -0.1330(12) 0.6247(11) 0.6539(3) 0.027(2) Uani 1 1 d . U . . .
Br3 Br 0.00804(19) 1.10510(18) 0.93882(4) 0.0181(3) Uani 1 1 d . . . . .
Br4 Br 0.13818(18) 1.15824(18) 0.82912(5) 0.0187(3) Uani 1 1 d . . . . .
C7 C 0.0030(17) 0.9340(16) 0.8976(4) 0.012(2) Uani 1 1 d . U . . .
C8 C 0.0624(18) 0.9532(17) 0.8523(4) 0.014(3) Uani 1 1 d . U . . .
C9 C 0.0597(17) 0.8205(18) 0.8248(4) 0.016(3) Uani 1 1 d . U . . .
C10 C 0.0000(18) 0.6686(18) 0.8392(5) 0.017(3) Uani 1 1 d . U . . .
C11 C -0.0659(19) 0.6523(19) 0.8838(5) 0.021(3) Uani 1 1 d . U . . .
C12 C -0.0606(17) 0.7824(17) 0.9122(4) 0.015(3) Uani 1 1 d . U . . .
F5 F 0.1219(12) 0.8371(12) 0.7813(3) 0.0234(19) Uani 1 1 d . U . . .
F6 F 0.0023(14) 0.5430(12) 0.8131(3) 0.032(2) Uani 1 1 d . U . . .
F7 F -0.1250(13) 0.5070(11) 0.8985(3) 0.031(2) Uani 1 1 d . U . . .
F8 F -0.1240(11) 0.7623(12) 0.9549(3) 0.0233(19) Uani 1 1 d . U . . .
C13 C 0.5981(19) 0.1604(18) 0.5961(5) 0.018(3) Uani 1 1 d . U . . .
C14 C 0.6722(18) 0.0147(18) 0.5789(4) 0.016(3) Uani 1 1 d . U . . .
H14 H 0.6750 -0.0831 0.5961 0.019 Uiso 1 1 calc R . . . .
C15 C 0.744(2) 0.0211(19) 0.5338(5) 0.022(3) Uani 1 1 d . U . . .
H15 H 0.7959 -0.0738 0.5213 0.026 Uiso 1 1 calc R . . . .
C16 C 0.7366(19) 0.1694(19) 0.5081(4) 0.018(3) Uani 1 1 d . U . . .
H16 H 0.7798 0.1694 0.4783 0.021 Uiso 1 1 calc R . . . .
C17 C 0.6678(19) 0.3147(18) 0.5256(4) 0.016(3) Uani 1 1 d . U . . .
H17 H 0.6700 0.4133 0.5088 0.019 Uiso 1 1 calc R . . . .
C18 C 0.5944(18) 0.3090(17) 0.5696(4) 0.014(3) Uani 1 1 d . U . . .
C19 C 0.5083(17) 0.4423(17) 0.5982(4) 0.013(2) Uani 1 1 d . U . . .
C20 C 0.4703(18) 0.6075(18) 0.5916(5) 0.017(3) Uani 1 1 d . U . . .
H20 H 0.4998 0.6613 0.5644 0.020 Uiso 1 1 calc R . . . .
C21 C 0.3830(18) 0.6945(19) 0.6281(5) 0.019(3) Uani 1 1 d . U . . .
H21 H 0.3527 0.8061 0.6240 0.023 Uiso 1 1 calc R . . . .
C22 C 0.3427(17) 0.6192(18) 0.6689(4) 0.015(3) Uani 1 1 d . U . . .
H22 H 0.2895 0.6804 0.6921 0.018 Uiso 1 1 calc R . . . .
C23 C 0.3818(18) 0.4492(17) 0.6758(4) 0.014(3) Uani 1 1 d . U . . .
C24 C 0.4662(17) 0.3657(17) 0.6400(4) 0.013(2) Uani 1 1 d . U . . .
C25 C 0.5154(17) 0.1950(17) 0.6412(4) 0.013(2) Uani 1 1 d . U . . .
C26 C 0.4796(18) 0.1020(18) 0.6789(4) 0.016(3) Uani 1 1 d . U . . .
H26 H 0.5102 -0.0103 0.6805 0.019 Uiso 1 1 calc R . . . .
C27 C 0.3920(18) 0.1853(18) 0.7164(5) 0.017(3) Uani 1 1 d . U . . .
H27 H 0.3643 0.1235 0.7424 0.020 Uiso 1 1 calc R . . . .
C28 C 0.3483(17) 0.3476(17) 0.7156(4) 0.013(2) Uani 1 1 d . U . . .
H28 H 0.2956 0.3952 0.7412 0.016 Uiso 1 1 calc R . . . .
C29 C 0.4174(18) 0.7861(17) 0.9250(4) 0.013(2) Uani 1 1 d . U . . .
C30 C 0.3581(17) 0.7784(18) 0.9706(4) 0.013(2) Uani 1 1 d . U . . .
H30 H 0.3658 0.8700 0.9887 0.016 Uiso 1 1 calc R . . . .
C31 C 0.289(2) 0.6337(19) 0.9882(5) 0.021(3) Uani 1 1 d . U . . .
H31 H 0.2486 0.6283 1.0182 0.025 Uiso 1 1 calc R . . . .
C32 C 0.2773(19) 0.4947(18) 0.9614(4) 0.017(3) Uani 1 1 d . U . . .
H32 H 0.2307 0.3977 0.9738 0.021 Uiso 1 1 calc R . . . .
C33 C 0.3367(19) 0.5009(19) 0.9155(5) 0.020(3) Uani 1 1 d . U . . .
H33 H 0.3277 0.4103 0.8971 0.024 Uiso 1 1 calc R . . . .
C34 C 0.4072(17) 0.6443(17) 0.8993(4) 0.013(2) Uani 1 1 d . U . . .
C35 C 0.4842(17) 0.6896(17) 0.8535(4) 0.012(2) Uani 1 1 d . U . . .
C36 C 0.5113(18) 0.6090(19) 0.8136(5) 0.019(3) Uani 1 1 d . U . . .
H36 H 0.4799 0.4993 0.8111 0.022 Uiso 1 1 calc R . . . .
C37 C 0.5886(19) 0.6977(19) 0.7762(5) 0.020(3) Uani 1 1 d . U . . .
H37 H 0.6081 0.6434 0.7491 0.023 Uiso 1 1 calc R . . . .
C38 C 0.6353(18) 0.8591(19) 0.7782(4) 0.017(3) Uani 1 1 d . U . . .
H38 H 0.6851 0.9122 0.7528 0.020 Uiso 1 1 calc R . . . .
C39 C 0.6081(18) 0.9466(18) 0.8192(5) 0.017(3) Uani 1 1 d . U . . .
C40 C 0.5305(16) 0.8555(16) 0.8551(4) 0.011(2) Uani 1 1 d . U . . .
C41 C 0.4966(17) 0.9214(17) 0.8987(4) 0.013(2) Uani 1 1 d . U . . .
C42 C 0.5355(18) 1.0827(17) 0.9057(4) 0.014(3) Uani 1 1 d . U . . .
H42 H 0.5118 1.1296 0.9336 0.017 Uiso 1 1 calc R . . . .
C43 C 0.6130(18) 1.1773(18) 0.8694(5) 0.018(3) Uani 1 1 d . U . . .
H43 H 0.6409 1.2866 0.8741 0.021 Uiso 1 1 calc R . . . .
C44 C 0.6474(19) 1.1129(19) 0.8281(5) 0.019(3) Uani 1 1 d . U . . .
H44 H 0.6976 1.1790 0.8052 0.023 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0172(7) 0.0369(9) 0.0093(6) -0.0092(6) 0.0038(5) 0.0035(6)
Br2 0.0184(7) 0.0187(7) 0.0275(8) 0.0033(6) 0.0027(5) 0.0022(5)
C1 0.008(5) 0.020(6) 0.015(5) -0.005(5) -0.001(4) -0.001(4)
C2 0.015(5) 0.016(5) 0.009(5) -0.005(5) 0.000(4) 0.001(5)
C3 0.014(5) 0.019(6) 0.016(5) -0.007(5) 0.001(4) 0.005(5)
C4 0.012(5) 0.034(7) 0.013(5) -0.004(5) -0.001(4) -0.007(5)
C5 0.021(6) 0.024(6) 0.014(5) 0.001(5) -0.004(5) -0.003(5)
C6 0.016(6) 0.018(6) 0.016(5) -0.005(5) -0.003(5) 0.002(5)
F1 0.027(5) 0.035(5) 0.018(4) -0.017(4) 0.005(3) 0.009(4)
F2 0.025(4) 0.055(6) 0.007(3) -0.001(4) 0.008(3) -0.007(4)
F3 0.029(5) 0.038(5) 0.030(5) 0.017(4) -0.004(4) -0.007(4)
F4 0.022(4) 0.026(5) 0.034(5) -0.006(4) -0.008(4) 0.001(4)
Br3 0.0189(7) 0.0260(7) 0.0093(6) -0.0084(5) 0.0011(5) 0.0043(5)
Br4 0.0159(6) 0.0252(7) 0.0143(6) 0.0046(5) 0.0033(5) 0.0007(5)
C7 0.013(4) 0.015(4) 0.008(4) -0.003(4) 0.002(3) 0.002(4)
C8 0.015(5) 0.016(5) 0.011(5) 0.000(5) -0.003(4) 0.005(5)
C9 0.009(5) 0.027(6) 0.011(5) -0.003(5) -0.008(4) 0.009(5)
C10 0.014(5) 0.020(6) 0.016(5) -0.008(5) -0.007(4) 0.008(5)
C11 0.016(6) 0.023(6) 0.025(6) 0.004(5) -0.004(5) 0.006(5)
C12 0.009(5) 0.021(6) 0.015(5) 0.000(5) -0.001(4) 0.002(5)
F5 0.025(4) 0.038(5) 0.006(3) -0.008(3) 0.001(3) 0.011(4)
F6 0.041(6) 0.028(5) 0.028(5) -0.014(4) -0.013(4) 0.011(4)
F7 0.034(5) 0.019(4) 0.040(5) 0.004(4) -0.004(4) -0.004(4)
F8 0.021(4) 0.038(5) 0.010(4) 0.006(4) 0.005(3) -0.002(4)
C13 0.016(6) 0.019(6) 0.019(6) -0.002(5) 0.000(5) -0.004(5)
C14 0.015(5) 0.019(6) 0.012(5) -0.002(5) 0.005(4) 0.003(5)
C15 0.022(6) 0.024(6) 0.020(6) -0.007(5) 0.000(5) 0.002(5)
C16 0.019(6) 0.030(6) 0.005(5) -0.006(5) 0.006(4) -0.002(5)
C17 0.021(6) 0.019(6) 0.008(5) -0.002(5) 0.003(4) -0.002(5)
C18 0.015(5) 0.018(5) 0.008(5) -0.005(5) 0.000(4) -0.001(5)
C19 0.012(5) 0.020(6) 0.007(5) -0.003(5) 0.002(4) 0.002(5)
C20 0.012(5) 0.023(6) 0.014(5) 0.001(5) 0.003(4) -0.003(5)
C21 0.012(5) 0.020(6) 0.026(6) -0.002(5) 0.002(5) 0.003(5)
C22 0.007(5) 0.024(6) 0.014(5) -0.005(5) -0.002(4) 0.005(5)
C23 0.013(5) 0.021(6) 0.008(5) -0.001(5) 0.001(4) -0.004(5)
C24 0.009(5) 0.023(6) 0.008(5) -0.003(5) -0.002(4) 0.001(5)
C25 0.011(5) 0.018(5) 0.011(5) -0.003(5) 0.000(4) 0.000(4)
C26 0.014(5) 0.021(6) 0.013(5) -0.003(5) -0.003(4) 0.003(5)
C27 0.014(5) 0.024(6) 0.013(5) 0.000(5) 0.002(4) 0.001(5)
C28 0.012(4) 0.019(4) 0.009(4) -0.004(4) 0.002(3) 0.002(4)
C29 0.017(5) 0.016(5) 0.007(5) -0.005(4) -0.002(4) 0.006(5)
C30 0.011(5) 0.023(6) 0.006(5) -0.001(5) 0.001(4) 0.001(5)
C31 0.022(6) 0.026(6) 0.015(5) -0.003(5) -0.002(5) 0.005(5)
C32 0.019(6) 0.021(6) 0.011(5) 0.002(5) 0.001(4) 0.003(5)
C33 0.017(6) 0.021(6) 0.023(6) -0.001(5) -0.001(5) 0.004(5)
C34 0.010(5) 0.021(6) 0.007(5) -0.001(5) -0.003(4) 0.006(4)
C35 0.008(5) 0.022(6) 0.006(5) -0.001(5) -0.001(4) 0.003(4)
C36 0.013(5) 0.024(6) 0.018(6) -0.006(5) -0.002(5) 0.006(5)
C37 0.019(6) 0.029(6) 0.011(5) -0.006(5) -0.002(4) 0.010(5)
C38 0.017(6) 0.027(6) 0.006(5) -0.003(5) 0.001(4) 0.007(5)
C39 0.009(5) 0.024(6) 0.018(6) 0.002(5) 0.008(4) 0.006(5)
C40 0.007(5) 0.018(5) 0.007(5) 0.000(4) 0.000(4) 0.007(4)
C41 0.011(5) 0.020(6) 0.007(5) -0.003(5) 0.004(4) 0.007(4)
C42 0.013(5) 0.019(6) 0.011(5) -0.006(5) 0.001(4) 0.006(5)
C43 0.013(5) 0.020(6) 0.020(6) 0.000(5) -0.003(5) 0.002(5)
C44 0.014(5) 0.025(6) 0.017(5) 0.002(5) -0.002(5) 0.001(5)
_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
Br1 C1 1.873(13) . ?
Br2 C2 1.874(13) . ?
C1 C2 1.383(19) . ?
C1 C6 1.384(19) . ?
C2 C3 1.391(18) . ?
C3 C4 1.39(2) . ?
C3 F1 1.325(16) . ?
C4 C5 1.38(2) . ?
C4 F2 1.323(15) . ?
C5 C6 1.386(19) . ?
C5 F3 1.329(17) . ?
C6 F4 1.349(17) . ?
Br3 C7 1.873(13) . ?
Br4 C8 1.877(14) . ?
C7 C8 1.407(17) . ?
C7 C12 1.384(19) . ?
C8 C9 1.37(2) . ?
C9 C10 1.37(2) . ?
C9 F5 1.362(15) . ?
C10 C11 1.40(2) . ?
C10 F6 1.292(17) . ?
C11 C12 1.37(2) . ?
C11 F7 1.327(17) . ?
C12 F8 1.345(15) . ?
C13 C14 1.39(2) . ?
C13 C18 1.419(19) . ?
C13 C25 1.483(19) . ?
C14 H14 0.9300 . ?
C14 C15 1.424(19) . ?
C15 H15 0.9300 . ?
C15 C16 1.41(2) . ?
C16 H16 0.9300 . ?
C16 C17 1.38(2) . ?
C17 H17 0.9300 . ?
C17 C18 1.399(17) . ?
C18 C19 1.505(19) . ?
C19 C20 1.37(2) . ?
C19 C24 1.402(17) . ?
C20 H20 0.9300 . ?
C20 C21 1.44(2) . ?
C21 H21 0.9300 . ?
C21 C22 1.370(19) . ?
C22 H22 0.9300 . ?
C22 C23 1.41(2) . ?
C23 C24 1.396(18) . ?
C23 C28 1.439(17) . ?
C24 C25 1.418(19) . ?
C25 C26 1.356(18) . ?
C26 H26 0.9300 . ?
C26 C27 1.443(19) . ?
C27 H27 0.9300 . ?
C27 C28 1.34(2) . ?
C28 H28 0.9300 . ?
C29 C30 1.412(17) . ?
C29 C34 1.398(19) . ?
C29 C41 1.456(19) . ?
C30 H30 0.9300 . ?
C30 C31 1.38(2) . ?
C31 H31 0.9300 . ?
C31 C32 1.40(2) . ?
C32 H32 0.9300 . ?
C32 C33 1.420(19) . ?
C33 H33 0.9300 . ?
C33 C34 1.36(2) . ?
C34 C35 1.500(17) . ?
C35 C36 1.373(19) . ?
C35 C40 1.399(19) . ?
C36 H36 0.9300 . ?
C36 C37 1.42(2) . ?
C37 H37 0.9300 . ?
C37 C38 1.37(2) . ?
C38 H38 0.9300 . ?
C38 C39 1.427(19) . ?
C39 C40 1.401(18) . ?
C39 C44 1.42(2) . ?
C40 C41 1.424(17) . ?
C41 C42 1.368(19) . ?
C42 H42 0.9300 . ?
C42 C43 1.424(19) . ?
C43 H43 0.9300 . ?
C43 C44 1.36(2) . ?
C44 H44 0.9300 . ?
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
C2 C1 Br1 122.6(10) . . ?
C2 C1 C6 119.8(12) . . ?
C6 C1 Br1 117.5(11) . . ?
C1 C2 Br2 122.3(10) . . ?
C1 C2 C3 119.9(12) . . ?
C3 C2 Br2 117.8(10) . . ?
C2 C3 C4 119.8(13) . . ?
F1 C3 C2 121.2(12) . . ?
F1 C3 C4 119.0(12) . . ?
C5 C4 C3 120.4(13) . . ?
F2 C4 C3 119.1(14) . . ?
F2 C4 C5 120.5(14) . . ?
C4 C5 C6 119.1(13) . . ?
F3 C5 C4 120.0(13) . . ?
F3 C5 C6 120.9(14) . . ?
C1 C6 C5 121.0(13) . . ?
F4 C6 C1 121.0(12) . . ?
F4 C6 C5 118.0(13) . . ?
C8 C7 Br3 122.5(10) . . ?
C12 C7 Br3 118.8(10) . . ?
C12 C7 C8 118.6(12) . . ?
C7 C8 Br4 121.1(10) . . ?
C9 C8 Br4 120.0(10) . . ?
C9 C8 C7 118.9(13) . . ?
C8 C9 C10 123.0(13) . . ?
F5 C9 C8 119.1(13) . . ?
F5 C9 C10 117.9(13) . . ?
C9 C10 C11 117.7(13) . . ?
F6 C10 C9 122.4(13) . . ?
F6 C10 C11 119.9(14) . . ?
C12 C11 C10 120.1(14) . . ?
F7 C11 C10 118.9(14) . . ?
F7 C11 C12 120.9(13) . . ?
C11 C12 C7 121.6(13) . . ?
F8 C12 C7 119.8(12) . . ?
F8 C12 C11 118.6(13) . . ?
C14 C13 C18 120.9(13) . . ?
C14 C13 C25 130.5(13) . . ?
C18 C13 C25 108.6(12) . . ?
C13 C14 H14 121.4 . . ?
C13 C14 C15 117.3(13) . . ?
C15 C14 H14 121.4 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.6(14) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 119.0 . . ?
C17 C16 C15 122.0(12) . . ?
C17 C16 H16 119.0 . . ?
C16 C17 H17 121.2 . . ?
C16 C17 C18 117.7(13) . . ?
C18 C17 H17 121.2 . . ?
C13 C18 C19 107.5(11) . . ?
C17 C18 C13 121.4(13) . . ?
C17 C18 C19 131.1(12) . . ?
C20 C19 C18 134.3(12) . . ?
C20 C19 C24 119.8(12) . . ?
C24 C19 C18 105.8(11) . . ?
C19 C20 H20 121.3 . . ?
C19 C20 C21 117.5(12) . . ?
C21 C20 H20 121.3 . . ?
C20 C21 H21 118.8 . . ?
C22 C21 C20 122.4(13) . . ?
C22 C21 H21 118.8 . . ?
C21 C22 H22 119.9 . . ?
C21 C22 C23 120.2(13) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 C28 128.6(13) . . ?
C24 C23 C22 116.9(12) . . ?
C24 C23 C28 114.5(12) . . ?
C19 C24 C25 112.4(12) . . ?
C23 C24 C19 123.2(13) . . ?
C23 C24 C25 124.4(12) . . ?
C24 C25 C13 105.7(11) . . ?
C26 C25 C13 134.5(13) . . ?
C26 C25 C24 119.8(12) . . ?
C25 C26 H26 121.6 . . ?
C25 C26 C27 116.9(13) . . ?
C27 C26 H26 121.6 . . ?
C26 C27 H27 118.3 . . ?
C28 C27 C26 123.4(13) . . ?
C28 C27 H27 118.3 . . ?
C23 C28 H28 119.5 . . ?
C27 C28 C23 121.1(12) . . ?
C27 C28 H28 119.5 . . ?
C30 C29 C41 130.1(12) . . ?
C34 C29 C30 118.4(12) . . ?
C34 C29 C41 111.4(11) . . ?
C29 C30 H30 120.3 . . ?
C31 C30 C29 119.3(13) . . ?
C31 C30 H30 120.3 . . ?
C30 C31 H31 119.6 . . ?
C30 C31 C32 120.9(13) . . ?
C32 C31 H31 119.6 . . ?
C31 C32 H32 119.8 . . ?
C31 C32 C33 120.3(13) . . ?
C33 C32 H32 119.8 . . ?
C32 C33 H33 121.2 . . ?
C34 C33 C32 117.5(14) . . ?
C34 C33 H33 121.2 . . ?
C29 C34 C35 105.8(12) . . ?
C33 C34 C29 123.5(12) . . ?
C33 C34 C35 130.7(13) . . ?
C36 C35 C34 135.1(13) . . ?
C36 C35 C40 118.5(12) . . ?
C40 C35 C34 106.4(11) . . ?
C35 C36 H36 120.9 . . ?
C35 C36 C37 118.2(14) . . ?
C37 C36 H36 120.9 . . ?
C36 C37 H37 118.6 . . ?
C38 C37 C36 122.9(13) . . ?
C38 C37 H37 118.6 . . ?
C37 C38 H38 119.9 . . ?
C37 C38 C39 120.3(13) . . ?
C39 C38 H38 119.9 . . ?
C40 C39 C38 115.2(13) . . ?
C40 C39 C44 116.1(13) . . ?
C44 C39 C38 128.7(13) . . ?
C35 C40 C39 125.0(12) . . ?
C35 C40 C41 112.0(11) . . ?
C39 C40 C41 123.0(13) . . ?
C40 C41 C29 104.4(12) . . ?
C42 C41 C29 136.7(12) . . ?
C42 C41 C40 118.9(12) . . ?
C41 C42 H42 120.6 . . ?
C41 C42 C43 118.7(12) . . ?
C43 C42 H42 120.6 . . ?
C42 C43 H43 119.0 . . ?
C44 C43 C42 122.0(14) . . ?
C44 C43 H43 119.0 . . ?
C39 C44 H44 119.4 . . ?
C43 C44 C39 121.2(13) . . ?
C43 C44 H44 119.4 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C1 C2 Br2 7.1(16) . . . . ?
Br1 C1 C2 C3 -174.7(10) . . . . ?
Br1 C1 C6 C5 177.3(11) . . . . ?
Br1 C1 C6 F4 -4.2(17) . . . . ?
Br2 C2 C3 C4 176.4(10) . . . . ?
Br2 C2 C3 F1 -1.8(18) . . . . ?
C1 C2 C3 C4 -2(2) . . . . ?
C1 C2 C3 F1 179.9(12) . . . . ?
C2 C1 C6 C5 1(2) . . . . ?
C2 C1 C6 F4 179.5(12) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
C2 C3 C4 F2 -179.4(12) . . . . ?
C3 C4 C5 C6 2(2) . . . . ?
C3 C4 C5 F3 -179.2(12) . . . . ?
C4 C5 C6 C1 -3(2) . . . . ?
C4 C5 C6 F4 178.5(12) . . . . ?
C6 C1 C2 Br2 -176.8(10) . . . . ?
C6 C1 C2 C3 1(2) . . . . ?
F1 C3 C4 C5 178.2(12) . . . . ?
F1 C3 C4 F2 -1(2) . . . . ?
F2 C4 C5 C6 -178.2(12) . . . . ?
F2 C4 C5 F3 0(2) . . . . ?
F3 C5 C6 C1 178.7(12) . . . . ?
F3 C5 C6 F4 0(2) . . . . ?
Br3 C7 C8 Br4 -3.9(16) . . . . ?
Br3 C7 C8 C9 177.9(10) . . . . ?
Br3 C7 C12 C11 -179.3(10) . . . . ?
Br3 C7 C12 F8 2.7(17) . . . . ?
Br4 C8 C9 C10 -177.7(10) . . . . ?
Br4 C8 C9 F5 3.7(16) . . . . ?
C7 C8 C9 C10 0(2) . . . . ?
C7 C8 C9 F5 -178.2(11) . . . . ?
C8 C7 C12 C11 0(2) . . . . ?
C8 C7 C12 F8 -177.8(11) . . . . ?
C8 C9 C10 C11 2.0(19) . . . . ?
C8 C9 C10 F6 -178.2(12) . . . . ?
C9 C10 C11 C12 -3(2) . . . . ?
C9 C10 C11 F7 179.7(12) . . . . ?
C10 C11 C12 C7 2(2) . . . . ?
C10 C11 C12 F8 -179.6(12) . . . . ?
C12 C7 C8 Br4 176.5(10) . . . . ?
C12 C7 C8 C9 -1.7(19) . . . . ?
F5 C9 C10 C11 -179.3(11) . . . . ?
F5 C9 C10 F6 0.4(19) . . . . ?
F6 C10 C11 C12 176.9(12) . . . . ?
F6 C10 C11 F7 0(2) . . . . ?
F7 C11 C12 C7 179.1(12) . . . . ?
F7 C11 C12 F8 -3(2) . . . . ?
C13 C14 C15 C16 -1(2) . . . . ?
C13 C18 C19 C20 179.2(15) . . . . ?
C13 C18 C19 C24 0.1(15) . . . . ?
C13 C25 C26 C27 -178.8(14) . . . . ?
C14 C13 C18 C17 -1(2) . . . . ?
C14 C13 C18 C19 -179.3(12) . . . . ?
C14 C13 C25 C24 179.0(14) . . . . ?
C14 C13 C25 C26 -2(3) . . . . ?
C14 C15 C16 C17 3(2) . . . . ?
C15 C16 C17 C18 -4(2) . . . . ?
C16 C17 C18 C13 3(2) . . . . ?
C16 C17 C18 C19 -179.5(13) . . . . ?
C17 C18 C19 C20 1(3) . . . . ?
C17 C18 C19 C24 -177.8(14) . . . . ?
C18 C13 C14 C15 0(2) . . . . ?
C18 C13 C25 C24 -0.5(15) . . . . ?
C18 C13 C25 C26 178.2(15) . . . . ?
C18 C19 C20 C21 179.4(14) . . . . ?
C18 C19 C24 C23 -179.2(12) . . . . ?
C18 C19 C24 C25 -0.5(15) . . . . ?
C19 C20 C21 C22 2(2) . . . . ?
C19 C24 C25 C13 0.6(15) . . . . ?
C19 C24 C25 C26 -178.4(12) . . . . ?
C20 C19 C24 C23 2(2) . . . . ?
C20 C19 C24 C25 -179.7(12) . . . . ?
C20 C21 C22 C23 -2(2) . . . . ?
C21 C22 C23 C24 1.7(19) . . . . ?
C21 C22 C23 C28 -179.1(13) . . . . ?
C22 C23 C24 C19 -1.5(19) . . . . ?
C22 C23 C24 C25 179.9(12) . . . . ?
C22 C23 C28 C27 179.0(14) . . . . ?
C23 C24 C25 C13 179.3(12) . . . . ?
C23 C24 C25 C26 0(2) . . . . ?
C24 C19 C20 C21 -1.6(19) . . . . ?
C24 C23 C28 C27 -1.8(19) . . . . ?
C24 C25 C26 C27 -0.2(19) . . . . ?
C25 C13 C14 C15 -179.4(14) . . . . ?
C25 C13 C18 C17 178.4(12) . . . . ?
C25 C13 C18 C19 0.2(15) . . . . ?
C25 C26 C27 C28 -1(2) . . . . ?
C26 C27 C28 C23 2(2) . . . . ?
C28 C23 C24 C19 179.2(12) . . . . ?
C28 C23 C24 C25 0.6(19) . . . . ?
C29 C30 C31 C32 0(2) . . . . ?
C29 C34 C35 C36 -179.3(15) . . . . ?
C29 C34 C35 C40 -1.3(13) . . . . ?
C29 C41 C42 C43 -178.8(14) . . . . ?
C30 C29 C34 C33 3(2) . . . . ?
C30 C29 C34 C35 -178.3(11) . . . . ?
C30 C29 C41 C40 179.3(13) . . . . ?
C30 C29 C41 C42 -3(3) . . . . ?
C30 C31 C32 C33 0(2) . . . . ?
C31 C32 C33 C34 1(2) . . . . ?
C32 C33 C34 C29 -3(2) . . . . ?
C32 C33 C34 C35 178.6(12) . . . . ?
C33 C34 C35 C36 0(2) . . . . ?
C33 C34 C35 C40 177.7(13) . . . . ?
C34 C29 C30 C31 -1.4(19) . . . . ?
C34 C29 C41 C40 1.4(14) . . . . ?
C34 C29 C41 C42 178.7(14) . . . . ?
C34 C35 C36 C37 179.1(13) . . . . ?
C34 C35 C40 C39 179.7(12) . . . . ?
C34 C35 C40 C41 2.2(14) . . . . ?
C35 C36 C37 C38 -1(2) . . . . ?
C35 C40 C41 C29 -2.2(14) . . . . ?
C35 C40 C41 C42 179.8(11) . . . . ?
C36 C35 C40 C39 -1.9(19) . . . . ?
C36 C35 C40 C41 -179.3(11) . . . . ?
C36 C37 C38 C39 0(2) . . . . ?
C37 C38 C39 C40 -0.7(19) . . . . ?
C37 C38 C39 C44 180.0(14) . . . . ?
C38 C39 C40 C35 1.6(19) . . . . ?
C38 C39 C40 C41 178.7(12) . . . . ?
C38 C39 C44 C43 -179.9(14) . . . . ?
C39 C40 C41 C29 -179.7(12) . . . . ?
C39 C40 C41 C42 2.4(19) . . . . ?
C40 C35 C36 C37 1.3(19) . . . . ?
C40 C39 C44 C43 0.8(19) . . . . ?
C40 C41 C42 C43 -1.7(18) . . . . ?
C41 C29 C30 C31 -179.3(13) . . . . ?
C41 C29 C34 C33 -179.1(12) . . . . ?
C41 C29 C34 C35 -0.1(14) . . . . ?
C41 C42 C43 C44 1(2) . . . . ?
C42 C43 C44 C39 0(2) . . . . ?
C44 C39 C40 C35 -179.0(12) . . . . ?
C44 C39 C40 C41 -1.9(19) . . . . ?
_shelx_res_file
;
20161202a.res created by SHELXL-2014/7
TITL 20161202a_a.res in P-1
REM Old TITL 20161202a in P-1 #2
REM SHELXT solution in P-1
REM R1 0.196, Rweak 0.052, Alpha 0.197, Orientation as input
REM Formula found by SHELXT: C20 F7 Br4
CELL 0.71073 7.405926 8.096605 29.631703 88.5097 88.4818 88.1856
ZERR 2 0.000784 0.000871 0.001304 0.006 0.006 0.0087
LATT 1
SFAC C H Br F
UNIT 88 40 8 16
ISOR 0.01 0.02 $C $F
ISOR 0.005 0.01 C7 C28 F2 F5
L.S. 4
PLAN 5
BOND $H
MORE -1
CONF
fmap 2
acta 52
OMIT 2 1 12
OMIT -2 -1 8
OMIT 3 -1 3
OMIT -2 1 23
OMIT 2 -1 18
OMIT 0 1 26
OMIT 4 1 5
OMIT 5 1 5
OMIT 2 1 13
OMIT 1 1 8
REM
REM
REM
WGHT 0.051600 81.377907
BASF 0.13001 0.13001 0.13001
FVAR 3.15943
BR1 3 -0.145109 0.347175 0.722345 11.00000 0.01719 0.03693 =
0.00928 -0.00923 0.00377 0.00350
BR2 3 0.001528 -0.011465 0.674591 11.00000 0.01839 0.01869 =
0.02747 0.00327 0.00267 0.00223
C1 1 -0.063670 0.336820 0.662087 11.00000 0.00766 0.02026 =
0.01460 -0.00503 -0.00128 -0.00131
C2 1 0.005907 0.192798 0.643428 11.00000 0.01505 0.01582 =
0.00880 -0.00501 -0.00006 0.00123
C3 1 0.077902 0.195924 0.599592 11.00000 0.01433 0.01894 =
0.01645 -0.00740 0.00114 0.00459
C4 1 0.074712 0.343440 0.574220 11.00000 0.01184 0.03391 =
0.01313 -0.00421 -0.00050 -0.00667
C5 1 0.000345 0.486443 0.592388 11.00000 0.02095 0.02386 =
0.01434 0.00133 -0.00359 -0.00348
C6 1 -0.064841 0.482656 0.636675 11.00000 0.01629 0.01840 =
0.01638 -0.00536 -0.00320 0.00192
F1 4 0.145644 0.059785 0.580875 11.00000 0.02741 0.03530 =
0.01847 -0.01681 0.00474 0.00891
F2 4 0.142283 0.344318 0.532435 11.00000 0.02460 0.05501 =
0.00738 -0.00083 0.00796 -0.00702
F3 4 -0.004087 0.626113 0.567793 11.00000 0.02868 0.03797 =
0.02995 0.01742 -0.00447 -0.00675
F4 4 -0.133034 0.624698 0.653910 11.00000 0.02179 0.02598 =
0.03374 -0.00606 -0.00797 0.00148
BR3 3 0.008043 1.105097 0.938824 11.00000 0.01889 0.02597 =
0.00933 -0.00842 0.00107 0.00432
BR4 3 0.138176 1.158244 0.829121 11.00000 0.01592 0.02525 =
0.01431 0.00459 0.00331 0.00072
C7 1 0.002953 0.934014 0.897585 11.00000 0.01268 0.01502 =
0.00784 -0.00318 0.00215 0.00237
C8 1 0.062448 0.953237 0.852332 11.00000 0.01453 0.01584 =
0.01073 -0.00002 -0.00255 0.00510
C9 1 0.059682 0.820502 0.824786 11.00000 0.00852 0.02748 =
0.01107 -0.00279 -0.00785 0.00862
C10 1 0.000020 0.668559 0.839151 11.00000 0.01407 0.01966 =
0.01621 -0.00761 -0.00686 0.00824
C11 1 -0.065857 0.652340 0.883849 11.00000 0.01637 0.02259 =
0.02458 0.00387 -0.00361 0.00578
C12 1 -0.060609 0.782377 0.912202 11.00000 0.00861 0.02058 =
0.01484 -0.00010 -0.00106 0.00189
F5 4 0.121917 0.837122 0.781302 11.00000 0.02532 0.03815 =
0.00637 -0.00838 0.00121 0.01084
F6 4 0.002299 0.543012 0.813108 11.00000 0.04065 0.02847 =
0.02821 -0.01353 -0.01337 0.01075
F7 4 -0.125008 0.506958 0.898491 11.00000 0.03426 0.01869 =
0.04038 0.00366 -0.00380 -0.00376
F8 4 -0.123972 0.762267 0.954875 11.00000 0.02144 0.03759 =
0.01029 0.00568 0.00475 -0.00198
C13 1 0.598086 0.160445 0.596124 11.00000 0.01555 0.01880 =
0.01922 -0.00194 0.00028 -0.00412
C14 1 0.672230 0.014683 0.578871 11.00000 0.01532 0.01885 =
0.01224 -0.00159 0.00473 0.00308
AFIX 43
H14 2 0.674965 -0.083080 0.596058 11.00000 -1.20000
AFIX 0
C15 1 0.743860 0.021091 0.533800 11.00000 0.02193 0.02374 =
0.01996 -0.00697 -0.00025 0.00202
AFIX 43
H15 2 0.795879 -0.073751 0.521251 11.00000 -1.20000
AFIX 0
C16 1 0.736650 0.169448 0.508113 11.00000 0.01863 0.02987 =
0.00513 -0.00618 0.00574 -0.00161
AFIX 43
H16 2 0.779756 0.169408 0.478349 11.00000 -1.20000
AFIX 0
C17 1 0.667792 0.314749 0.525639 11.00000 0.02056 0.01874 =
0.00761 -0.00215 0.00334 -0.00173
AFIX 43
H17 2 0.669969 0.413320 0.508834 11.00000 -1.20000
AFIX 0
C18 1 0.594397 0.308992 0.569621 11.00000 0.01489 0.01822 =
0.00782 -0.00532 0.00009 -0.00087
C19 1 0.508317 0.442284 0.598236 11.00000 0.01172 0.01996 =
0.00724 -0.00268 0.00171 0.00228
C20 1 0.470269 0.607474 0.591562 11.00000 0.01243 0.02316 =
0.01418 0.00147 0.00317 -0.00336
AFIX 43
H20 2 0.499803 0.661316 0.564384 11.00000 -1.20000
AFIX 0
C21 1 0.382971 0.694527 0.628141 11.00000 0.01166 0.01981 =
0.02561 -0.00210 0.00169 0.00270
AFIX 43
H21 2 0.352674 0.806130 0.623978 11.00000 -1.20000
AFIX 0
C22 1 0.342723 0.619153 0.668930 11.00000 0.00704 0.02398 =
0.01406 -0.00527 -0.00226 0.00518
AFIX 43
H22 2 0.289450 0.680412 0.692122 11.00000 -1.20000
AFIX 0
C23 1 0.381782 0.449154 0.675850 11.00000 0.01324 0.02126 =
0.00837 -0.00127 0.00123 -0.00359
C24 1 0.466217 0.365733 0.640023 11.00000 0.00883 0.02291 =
0.00798 -0.00347 -0.00197 0.00144
C25 1 0.515444 0.195001 0.641181 11.00000 0.01131 0.01756 =
0.01106 -0.00293 -0.00020 0.00003
C26 1 0.479648 0.101975 0.678893 11.00000 0.01406 0.02068 =
0.01325 -0.00263 -0.00262 0.00279
AFIX 43
H26 2 0.510184 -0.010285 0.680529 11.00000 -1.20000
AFIX 0
C27 1 0.391969 0.185300 0.716363 11.00000 0.01380 0.02377 =
0.01285 0.00019 0.00208 0.00062
AFIX 43
H27 2 0.364275 0.123454 0.742374 11.00000 -1.20000
AFIX 0
C28 1 0.348318 0.347617 0.715590 11.00000 0.01206 0.01896 =
0.00881 -0.00444 0.00225 0.00165
AFIX 43
H28 2 0.295592 0.395178 0.741162 11.00000 -1.20000
AFIX 0
C29 1 0.417432 0.786106 0.924985 11.00000 0.01710 0.01568 =
0.00729 -0.00495 -0.00151 0.00600
C30 1 0.358084 0.778418 0.970647 11.00000 0.01148 0.02274 =
0.00554 -0.00108 0.00061 0.00120
AFIX 43
H30 2 0.365799 0.870047 0.988704 11.00000 -1.20000
AFIX 0
C31 1 0.288570 0.633660 0.988193 11.00000 0.02156 0.02618 =
0.01493 -0.00306 -0.00188 0.00456
AFIX 43
H31 2 0.248639 0.628344 1.018202 11.00000 -1.20000
AFIX 0
C32 1 0.277322 0.494653 0.961437 11.00000 0.01885 0.02064 =
0.01150 0.00169 0.00055 0.00304
AFIX 43
H32 2 0.230725 0.397719 0.973807 11.00000 -1.20000
AFIX 0
C33 1 0.336717 0.500921 0.915495 11.00000 0.01666 0.02096 =
0.02264 -0.00107 -0.00096 0.00401
AFIX 43
H33 2 0.327712 0.410258 0.897140 11.00000 -1.20000
AFIX 0
C34 1 0.407208 0.644331 0.899345 11.00000 0.00957 0.02134 =
0.00667 -0.00143 -0.00294 0.00623
C35 1 0.484232 0.689645 0.853520 11.00000 0.00771 0.02245 =
0.00589 -0.00150 -0.00129 0.00262
C36 1 0.511294 0.608969 0.813588 11.00000 0.01336 0.02413 =
0.01847 -0.00633 -0.00160 0.00635
AFIX 43
H36 2 0.479949 0.499326 0.811076 11.00000 -1.20000
AFIX 0
C37 1 0.588577 0.697690 0.776172 11.00000 0.01881 0.02891 =
0.01063 -0.00600 -0.00178 0.00981
AFIX 43
H37 2 0.608124 0.643393 0.749120 11.00000 -1.20000
AFIX 0
C38 1 0.635335 0.859108 0.778229 11.00000 0.01673 0.02694 =
0.00642 -0.00341 0.00115 0.00695
AFIX 43
H38 2 0.685110 0.912225 0.752850 11.00000 -1.20000
AFIX 0
C39 1 0.608097 0.946588 0.819181 11.00000 0.00943 0.02427 =
0.01761 0.00164 0.00775 0.00624
C40 1 0.530459 0.855498 0.855128 11.00000 0.00666 0.01842 =
0.00667 -0.00007 -0.00049 0.00656
C41 1 0.496633 0.921396 0.898744 11.00000 0.01056 0.01994 =
0.00653 -0.00312 0.00372 0.00701
C42 1 0.535511 1.082668 0.905705 11.00000 0.01251 0.01939 =
0.01116 -0.00590 0.00077 0.00610
AFIX 43
H42 2 0.511778 1.129611 0.933639 11.00000 -1.20000
AFIX 0
C43 1 0.612991 1.177292 0.869380 11.00000 0.01325 0.02009 =
0.02021 0.00047 -0.00312 0.00194
AFIX 43
H43 2 0.640921 1.286583 0.874097 11.00000 -1.20000
AFIX 0
C44 1 0.647376 1.112892 0.828056 11.00000 0.01417 0.02534 =
0.01703 0.00203 -0.00214 0.00106
AFIX 43
H44 2 0.697566 1.178962 0.805162 11.00000 -1.20000
AFIX 0
HKLF 5
REM 20161202a_a.res in P-1
REM R1 = 0.1096 for 6311 Fo > 4sig(Fo) and 0.1376 for all 8538 data
REM 508 parameters refined using 312 restraints
END
WGHT 0.0516 81.4048
REM Highest difference peak 2.973, deepest hole -2.507, 1-sigma level 0.382
Q1 1 -0.1411 0.4941 0.7229 11.00000 0.05 2.97
Q2 1 0.0051 1.2454 0.9405 11.00000 0.05 2.60
Q3 1 0.1406 1.0219 0.8299 11.00000 0.05 2.28
Q4 1 -0.0032 0.9678 0.9349 11.00000 0.05 2.28
Q5 1 -0.0009 0.1252 0.6775 11.00000 0.05 2.24
;
_shelx_res_checksum 900
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.452
_oxdiff_exptl_absorpt_empirical_full_min 0.555
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.61(14)
2 0.13(8)
3 0.13(8)
4 0.13(8)
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_20161228b
_database_code_depnum_ccdc_archive 'CCDC 1547629'
_audit_update_record
;
2017-05-03 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_audit_creation_date 2016-12-31
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C6 F4 I2, C16 H10'
_chemical_formula_sum 'C22 H10 F4 I2'
_chemical_formula_weight 604.10
_chemical_melting_point ?
_chemical_oxdiff_formula c1h1f1i1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 15.2963(3)
_cell_length_b 18.1009(4)
_cell_length_c 30.4800(5)
_cell_angle_alpha 99.2518(16)
_cell_angle_beta 90.4052(15)
_cell_angle_gamma 114.420(2)
_cell_volume 7558.8(3)
_cell_formula_units_Z 16
_cell_measurement_reflns_used 66605
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 29.6660
_cell_measurement_theta_min 3.5980
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 3.371
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.58683
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 2.123
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 4544
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.3
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0342
_diffrn_reflns_av_unetI/netI 0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.825
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -42
_diffrn_reflns_number 75567
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 29.937
_diffrn_reflns_theta_min 3.163
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.825
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -27.00 25.00 1.00 10.00 -- 12.76 -57.00 -30.00 52
2 \w -11.00 53.00 1.00 10.00 -- 12.76 -99.00 60.00 64
3 \w -11.00 29.00 1.00 10.00 -- -11.04 -99.00 90.00 40
4 \w -15.00 13.00 1.00 10.00 -- 12.76 -37.00 60.00 28
5 \w -12.00 71.00 1.00 10.00 -- 12.76 37.00 -60.00 83
6 \w -21.00 88.00 1.00 10.00 -- 12.76 19.00-150.00 109
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0256758000
_diffrn_orient_matrix_UB_12 -0.0228290000
_diffrn_orient_matrix_UB_13 -0.0207482000
_diffrn_orient_matrix_UB_21 -0.0240828000
_diffrn_orient_matrix_UB_22 0.0262020000
_diffrn_orient_matrix_UB_23 0.0005532000
_diffrn_orient_matrix_UB_31 0.0370341000
_diffrn_orient_matrix_UB_32 0.0265768000
_diffrn_orient_matrix_UB_33 -0.0113520000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 28572
_reflns_number_total 36197
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 2.457
_refine_diff_density_min -3.125
_refine_diff_density_rms 0.144
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.113
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 2017
_refine_ls_number_reflns 36197
_refine_ls_number_restraints 1056
_refine_ls_R_factor_all 0.0640
_refine_ls_R_factor_gt 0.0449
_refine_ls_restrained_S_all 1.118
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+7.1132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0733
_refine_ls_wR_factor_ref 0.0820
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq,
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq,
Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq,
Uanis(C89) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92)
\\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C95) \\sim Ueq,
Uanis(C96) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C99)
\\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq,
Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C111) \\sim Ueq,
Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(C115) \\sim Ueq, Uanis(C116) \\sim Ueq, Uanis(C117) \\sim Ueq,
Uanis(C118) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq,
Uanis(C121) \\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(C123) \\sim Ueq,
Uanis(C124) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C126) \\sim Ueq,
Uanis(C127) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C129) \\sim Ueq,
Uanis(C130) \\sim Ueq, Uanis(C131) \\sim Ueq, Uanis(C132) \\sim Ueq,
Uanis(C133) \\sim Ueq, Uanis(C134) \\sim Ueq, Uanis(C135) \\sim Ueq,
Uanis(C136) \\sim Ueq, Uanis(C137) \\sim Ueq, Uanis(C138) \\sim Ueq,
Uanis(C139) \\sim Ueq, Uanis(C140) \\sim Ueq, Uanis(C141) \\sim Ueq,
Uanis(C142) \\sim Ueq, Uanis(C143) \\sim Ueq, Uanis(C144) \\sim Ueq,
Uanis(C145) \\sim Ueq, Uanis(C146) \\sim Ueq, Uanis(C147) \\sim Ueq,
Uanis(C148) \\sim Ueq, Uanis(C149) \\sim Ueq, Uanis(C150) \\sim Ueq,
Uanis(C151) \\sim Ueq, Uanis(C152) \\sim Ueq, Uanis(C153) \\sim Ueq,
Uanis(C154) \\sim Ueq, Uanis(C155) \\sim Ueq, Uanis(C156) \\sim Ueq,
Uanis(C157) \\sim Ueq, Uanis(C158) \\sim Ueq, Uanis(C159) \\sim Ueq,
Uanis(C160) \\sim Ueq, Uanis(C161) \\sim Ueq, Uanis(C162) \\sim Ueq,
Uanis(C163) \\sim Ueq, Uanis(C164) \\sim Ueq, Uanis(C165) \\sim Ueq,
Uanis(C166) \\sim Ueq, Uanis(C167) \\sim Ueq, Uanis(C168) \\sim Ueq,
Uanis(C169) \\sim Ueq, Uanis(C170) \\sim Ueq, Uanis(C171) \\sim Ueq,
Uanis(C172) \\sim Ueq, Uanis(C173) \\sim Ueq, Uanis(C174) \\sim Ueq,
Uanis(C175) \\sim Ueq, Uanis(C176) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
C50(H50), C51(H51), C52(H52), C53(H53), C56(H56), C57(H57), C58(H58),
C60(H60), C61(H61), C62(H62), C66(H66), C67(H67), C68(H68), C69(H69), C72(H72),
C73(H73), C74(H74), C76(H76), C77(H77), C78(H78), C82(H82), C83(H83),
C84(H84), C85(H85), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93), C94(H94),
C98(H98), C99(H99), C100(H100), C101(H101), C104(H104), C105(H105),
C106(H106), C108(H108), C109(H109), C110(H110), C114(H114), C115(H115),
C116(H116), C117(H117), C120(H120), C121(H121), C122(H122), C124(H124),
C125(H125), C126(H126), C130(H130), C131(H131), C132(H132), C133(H133),
C136(H136), C137(H137), C138(H138), C140(H140), C141(H141), C142(H142),
C146(H146), C147(H147), C148(H148), C149(H149), C152(H152), C153(H153),
C154(H154), C156(H156), C157(H157), C158(H158), C162(H162), C163(H163),
C164(H164), C165(H165), C168(H168), C169(H169), C170(H170), C172(H172),
C173(H173), C174(H174)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
C1 C 0.7099(3) 1.0382(3) 0.38716(14) 0.0190(10) Uani 1 1 d . U . . .
C2 C 0.7876(3) 1.0245(3) 0.36927(14) 0.0188(10) Uani 1 1 d . U . . .
C3 C 0.7705(3) 0.9481(3) 0.34499(14) 0.0196(10) Uani 1 1 d . U . . .
C4 C 0.6805(4) 0.8845(3) 0.33848(14) 0.0212(10) Uani 1 1 d . U . . .
C5 C 0.6041(3) 0.8975(3) 0.35610(15) 0.0241(11) Uani 1 1 d . U . . .
C6 C 0.6198(3) 0.9740(3) 0.38024(14) 0.0207(10) Uani 1 1 d . U . . .
C7 C 0.2631(3) 0.0662(3) 0.38571(13) 0.0183(10) Uani 1 1 d . U . . .
C8 C 0.3616(3) 0.1076(3) 0.38123(15) 0.0231(10) Uani 1 1 d . U . . .
C9 C 0.4087(3) 0.0648(3) 0.35787(15) 0.0252(11) Uani 1 1 d . U . . .
C10 C 0.3618(4) -0.0172(3) 0.33972(15) 0.0277(12) Uani 1 1 d . U . . .
C11 C 0.2653(4) -0.0584(3) 0.34433(15) 0.0287(12) Uani 1 1 d . U . . .
C12 C 0.2161(4) -0.0166(3) 0.36667(15) 0.0261(11) Uani 1 1 d . U . . .
C13 C 0.2535(3) 0.4328(3) 0.12552(14) 0.0207(10) Uani 1 1 d . U . . .
C14 C 0.1622(3) 0.4070(3) 0.10379(14) 0.0206(10) Uani 1 1 d . U . . .
C15 C 0.1224(3) 0.4632(3) 0.10487(14) 0.0214(10) Uani 1 1 d . U . . .
C16 C 0.1693(4) 0.5431(3) 0.12797(15) 0.0242(11) Uani 1 1 d . U . . .
C17 C 0.2591(4) 0.5685(3) 0.14865(15) 0.0250(11) Uani 1 1 d . U . . .
C18 C 0.3003(3) 0.5134(3) 0.14734(14) 0.0216(10) Uani 1 1 d . U . . .
C19 C 0.2522(3) 0.4608(3) 0.37683(13) 0.0200(10) Uani 1 1 d . U . . .
C20 C 0.1579(3) 0.4402(3) 0.36073(14) 0.0218(10) Uani 1 1 d . U . . .
C21 C 0.1305(3) 0.5022(3) 0.35684(14) 0.0227(11) Uani 1 1 d . U . . .
C22 C 0.1937(4) 0.5839(3) 0.36835(14) 0.0214(10) Uani 1 1 d . U . . .
C23 C 0.2867(4) 0.6044(3) 0.38305(14) 0.0220(11) Uani 1 1 d . U . . .
C24 C 0.3159(3) 0.5426(3) 0.38712(14) 0.0201(10) Uani 1 1 d . U . . .
C25 C 0.8109(3) 0.4450(3) 0.13341(14) 0.0195(10) Uani 1 1 d . U . . .
C26 C 0.7406(4) 0.4722(3) 0.12382(15) 0.0276(12) Uani 1 1 d . U . . .
C27 C 0.7574(5) 0.5535(4) 0.13981(18) 0.0384(15) Uani 1 1 d . U . . .
C28 C 0.8417(5) 0.6075(3) 0.16425(17) 0.0374(15) Uani 1 1 d . U . . .
C29 C 0.9106(4) 0.5813(3) 0.17333(15) 0.0294(12) Uani 1 1 d . U . . .
C30 C 0.8957(4) 0.5012(3) 0.15821(14) 0.0217(10) Uani 1 1 d . U . . .
C31 C 0.7873(4) 0.4713(3) 0.38734(14) 0.0201(10) Uani 1 1 d . U . . .
C32 C 0.7303(3) 0.5102(3) 0.37721(14) 0.0197(10) Uani 1 1 d . U . . .
C33 C 0.7694(4) 0.5951(3) 0.38380(14) 0.0214(10) Uani 1 1 d . U . . .
C34 C 0.8633(4) 0.6418(3) 0.40007(14) 0.0209(10) Uani 1 1 d . U . . .
C35 C 0.9213(4) 0.6040(3) 0.41004(15) 0.0252(11) Uani 1 1 d . U . . .
C36 C 0.8819(4) 0.5190(3) 0.40390(14) 0.0239(11) Uani 1 1 d . U . . .
C37 C 0.7017(3) 1.0053(3) 0.12975(14) 0.0192(10) Uani 1 1 d . U . . .
C38 C 0.7776(3) 0.9866(3) 0.11293(14) 0.0203(10) Uani 1 1 d . U . . .
C39 C 0.7613(3) 0.9054(3) 0.09942(14) 0.0221(10) Uani 1 1 d . U . . .
C40 C 0.6723(4) 0.8418(3) 0.10187(15) 0.0227(10) Uani 1 1 d . U . . .
C41 C 0.5986(3) 0.8605(3) 0.11779(14) 0.0236(11) Uani 1 1 d . U . . .
C42 C 0.6139(3) 0.9407(3) 0.13168(14) 0.0225(11) Uani 1 1 d . U . . .
C43 C 0.2640(3) 1.0431(3) 0.13021(14) 0.0207(10) Uani 1 1 d . U . . .
C44 C 0.3579(4) 1.0671(3) 0.11797(14) 0.0221(10) Uani 1 1 d . U . . .
C45 C 0.3869(4) 1.0054(3) 0.10051(14) 0.0214(10) Uani 1 1 d . U . . .
C46 C 0.3284(4) 0.9239(3) 0.09684(14) 0.0232(11) Uani 1 1 d . U . . .
C47 C 0.2352(4) 0.9010(3) 0.10864(14) 0.0222(10) Uani 1 1 d . U . . .
C48 C 0.2043(3) 0.9605(3) 0.12537(14) 0.0232(11) Uani 1 1 d . U . . .
C49 C 0.6874(4) 1.0135(3) 0.51809(15) 0.0249(11) Uani 1 1 d . U . . .
C50 C 0.6400(4) 1.0530(4) 0.54424(17) 0.0357(14) Uani 1 1 d . U . . .
H50 H 0.5735 1.0277 0.5451 0.043 Uiso 1 1 calc R . . . .
C51 C 0.6933(5) 1.1309(4) 0.56897(18) 0.0422(15) Uani 1 1 d . U . . .
H51 H 0.6618 1.1578 0.5864 0.051 Uiso 1 1 calc R . . . .
C52 C 0.7910(5) 1.1691(3) 0.56826(17) 0.0421(15) Uani 1 1 d . U . . .
H52 H 0.8248 1.2215 0.5851 0.050 Uiso 1 1 calc R . . . .
C53 C 0.8411(4) 1.1305(3) 0.54252(16) 0.0331(13) Uani 1 1 d . U . . .
H53 H 0.9079 1.1562 0.5427 0.040 Uiso 1 1 calc R . . . .
C54 C 0.7893(4) 1.0532(3) 0.51679(15) 0.0254(11) Uani 1 1 d . U . . .
C55 C 0.8191(3) 0.9981(3) 0.48614(15) 0.0232(11) Uani 1 1 d . U . . .
C56 C 0.9039(4) 1.0012(3) 0.47033(16) 0.0303(12) Uani 1 1 d . U . . .
H56 H 0.9614 1.0475 0.4795 0.036 Uiso 1 1 calc R . . . .
C57 C 0.9028(4) 0.9329(4) 0.43989(17) 0.0358(14) Uani 1 1 d . U . . .
H57 H 0.9607 0.9350 0.4296 0.043 Uiso 1 1 calc R . . . .
C58 C 0.8201(4) 0.8642(3) 0.42501(17) 0.0334(13) Uani 1 1 d . U . . .
H58 H 0.8227 0.8210 0.4048 0.040 Uiso 1 1 calc R . . . .
C59 C 0.7300(4) 0.8580(3) 0.44014(16) 0.0289(12) Uani 1 1 d . U . . .
C60 C 0.6378(4) 0.7914(3) 0.42919(17) 0.0373(14) Uani 1 1 d . U . . .
H60 H 0.6310 0.7442 0.4094 0.045 Uiso 1 1 calc R . . . .
C61 C 0.5591(4) 0.7966(3) 0.44759(17) 0.0376(14) Uani 1 1 d . U . . .
H61 H 0.4995 0.7519 0.4401 0.045 Uiso 1 1 calc R . . . .
C62 C 0.5641(4) 0.8668(3) 0.47751(18) 0.0356(13) Uani 1 1 d . U . . .
H62 H 0.5088 0.8687 0.4891 0.043 Uiso 1 1 calc R . . . .
C63 C 0.6523(4) 0.9322(3) 0.48912(16) 0.0257(11) Uani 1 1 d . U . . .
C64 C 0.7336(3) 0.9262(3) 0.47036(15) 0.0222(10) Uani 1 1 d . U . . .
C65 C 0.8118(3) 0.4719(3) 0.51330(13) 0.0179(10) Uani 1 1 d . U . . .
C66 C 0.8501(4) 0.4177(3) 0.52048(13) 0.0212(10) Uani 1 1 d . U . . .
H66 H 0.9156 0.4365 0.5281 0.025 Uiso 1 1 calc R . . . .
C67 C 0.7890(4) 0.3346(3) 0.51607(15) 0.0288(12) Uani 1 1 d . U . . .
H67 H 0.8140 0.2973 0.5205 0.035 Uiso 1 1 calc R . . . .
C68 C 0.6919(4) 0.3068(3) 0.50525(15) 0.0259(11) Uani 1 1 d . U . . .
H68 H 0.6520 0.2510 0.5030 0.031 Uiso 1 1 calc R . . . .
C69 C 0.6524(4) 0.3606(3) 0.49761(14) 0.0235(11) Uani 1 1 d . U . . .
H69 H 0.5866 0.3414 0.4905 0.028 Uiso 1 1 calc R . . . .
C70 C 0.7130(3) 0.4435(3) 0.50075(13) 0.0176(10) Uani 1 1 d . U . . .
C71 C 0.6938(3) 0.5149(3) 0.49412(13) 0.0176(10) Uani 1 1 d . U . . .
C72 C 0.6146(4) 0.5259(3) 0.48066(14) 0.0247(11) Uani 1 1 d . U . . .
H72 H 0.5548 0.4814 0.4734 0.030 Uiso 1 1 calc R . . . .
C73 C 0.6267(4) 0.6073(3) 0.47821(15) 0.0310(12) Uani 1 1 d . U . . .
H73 H 0.5735 0.6153 0.4693 0.037 Uiso 1 1 calc R . . . .
C74 C 0.7134(4) 0.6742(3) 0.48840(15) 0.0282(12) Uani 1 1 d . U . . .
H74 H 0.7177 0.7264 0.4868 0.034 Uiso 1 1 calc R . . . .
C75 C 0.7968(4) 0.6649(3) 0.50131(14) 0.0232(11) Uani 1 1 d . U . . .
C76 C 0.8925(4) 0.7260(3) 0.51154(15) 0.0295(12) Uani 1 1 d . U . . .
H76 H 0.9062 0.7805 0.5098 0.035 Uiso 1 1 calc R . . . .
C77 C 0.9652(4) 0.7058(3) 0.52394(15) 0.0281(12) Uani 1 1 d . U . . .
H77 H 1.0271 0.7474 0.5308 0.034 Uiso 1 1 calc R . . . .
C78 C 0.9492(3) 0.6234(3) 0.52676(14) 0.0216(10) Uani 1 1 d . U . . .
H78 H 0.9992 0.6110 0.5356 0.026 Uiso 1 1 calc R . . . .
C79 C 0.8573(3) 0.5629(3) 0.51590(13) 0.0171(10) Uani 1 1 d . U . . .
C80 C 0.7833(3) 0.5844(3) 0.50349(13) 0.0177(10) Uani 1 1 d . U . . .
C81 C 0.6803(3) 1.0072(3) 0.25745(13) 0.0177(10) Uani 1 1 d . U . . .
C82 C 0.6353(4) 1.0549(3) 0.27722(14) 0.0230(10) Uani 1 1 d . U . . .
H82 H 0.5698 1.0307 0.2811 0.028 Uiso 1 1 calc R . . . .
C83 C 0.6882(4) 1.1387(3) 0.29123(16) 0.0324(12) Uani 1 1 d . U . . .
H83 H 0.6580 1.1710 0.3044 0.039 Uiso 1 1 calc R . . . .
C84 C 0.7852(4) 1.1747(3) 0.28589(16) 0.0341(13) Uani 1 1 d . U . . .
H84 H 0.8200 1.2310 0.2960 0.041 Uiso 1 1 calc R . . . .
C85 C 0.8323(4) 1.1286(3) 0.26567(16) 0.0344(13) Uani 1 1 d . U . . .
H85 H 0.8978 1.1538 0.2620 0.041 Uiso 1 1 calc R . . . .
C86 C 0.7804(4) 1.0449(3) 0.25113(14) 0.0231(11) Uani 1 1 d . U . . .
C87 C 0.8088(4) 0.9809(4) 0.22901(15) 0.0353(13) Uani 1 1 d . U . . .
C88 C 0.8923(5) 0.9801(5) 0.21304(18) 0.0566(19) Uani 1 1 d . U . . .
H88 H 0.9485 1.0284 0.2159 0.068 Uiso 1 1 calc R . . . .
C89 C 0.8904(7) 0.9045(6) 0.1923(2) 0.077(2) Uani 1 1 d . U . . .
H89 H 0.9469 0.9038 0.1818 0.093 Uiso 1 1 calc R . . . .
C90 C 0.8118(7) 0.8338(5) 0.1870(2) 0.073(2) Uani 1 1 d . U . . .
H90 H 0.8154 0.7858 0.1727 0.088 Uiso 1 1 calc R . . . .
C91 C 0.7205(6) 0.8291(4) 0.20279(19) 0.0547(18) Uani 1 1 d . U . . .
C92 C 0.6300(7) 0.7630(4) 0.2001(2) 0.065(2) Uani 1 1 d . U . . .
H92 H 0.6230 0.7107 0.1869 0.079 Uiso 1 1 calc R . . . .
C93 C 0.5513(6) 0.7725(4) 0.21613(19) 0.060(2) Uani 1 1 d . U . . .
H93 H 0.4927 0.7265 0.2137 0.072 Uiso 1 1 calc R . . . .
C94 C 0.5570(4) 0.8516(3) 0.23654(16) 0.0387(14) Uani 1 1 d . U . . .
H94 H 0.5030 0.8575 0.2472 0.046 Uiso 1 1 calc R . . . .
C95 C 0.6443(4) 0.9184(3) 0.23984(14) 0.0235(11) Uani 1 1 d . U . . .
C96 C 0.7246(4) 0.9065(3) 0.22322(15) 0.0321(13) Uani 1 1 d . U . . .
C97 C 0.8153(4) 0.6267(3) 0.27523(15) 0.0304(13) Uani 1 1 d . U . . .
C98 C 0.8474(5) 0.7119(4) 0.28718(17) 0.0435(15) Uani 1 1 d . U . . .
H98 H 0.8078 0.7374 0.2816 0.052 Uiso 1 1 calc R . . . .
C99 C 0.9397(5) 0.7577(4) 0.30762(19) 0.0522(18) Uani 1 1 d . U . . .
H99 H 0.9624 0.8147 0.3158 0.063 Uiso 1 1 calc R . . . .
C100 C 0.9982(5) 0.7195(4) 0.31592(19) 0.0554(19) Uani 1 1 d . U . . .
H100 H 1.0597 0.7516 0.3298 0.067 Uiso 1 1 calc R . . . .
C101 C 0.9682(4) 0.6351(4) 0.30430(17) 0.0413(15) Uani 1 1 d . U . . .
H101 H 1.0087 0.6105 0.3102 0.050 Uiso 1 1 calc R . . . .
C102 C 0.8759(4) 0.5878(3) 0.28356(15) 0.0301(12) Uani 1 1 d . U . . .
C103 C 0.8240(4) 0.4998(3) 0.26701(15) 0.0262(11) Uani 1 1 d . U . . .
C104 C 0.8452(4) 0.4309(4) 0.26456(16) 0.0344(13) Uani 1 1 d . U . . .
H104 H 0.9045 0.4361 0.2759 0.041 Uiso 1 1 calc R . . . .
C105 C 0.7739(4) 0.3540(3) 0.24433(16) 0.0356(13) Uani 1 1 d . U . . .
H105 H 0.7870 0.3079 0.2430 0.043 Uiso 1 1 calc R . . . .
C106 C 0.6859(4) 0.3429(3) 0.22640(16) 0.0359(14) Uani 1 1 d . U . . .
H106 H 0.6419 0.2905 0.2129 0.043 Uiso 1 1 calc R . . . .
C107 C 0.6617(4) 0.4109(3) 0.22835(15) 0.0310(12) Uani 1 1 d . U . . .
C108 C 0.5755(4) 0.4116(3) 0.21134(15) 0.0303(12) Uani 1 1 d . U . . .
H108 H 0.5249 0.3626 0.1979 0.036 Uiso 1 1 calc R . . . .
C109 C 0.5671(4) 0.4852(4) 0.21485(16) 0.0351(13) Uani 1 1 d . U . . .
H109 H 0.5106 0.4848 0.2031 0.042 Uiso 1 1 calc R . . . .
C110 C 0.6409(4) 0.5613(4) 0.23565(16) 0.0334(13) Uani 1 1 d . U . . .
H110 H 0.6330 0.6100 0.2377 0.040 Uiso 1 1 calc R . . . .
C111 C 0.7244(4) 0.5620(3) 0.25276(15) 0.0262(11) Uani 1 1 d . U . . .
C112 C 0.7340(4) 0.4865(3) 0.24856(14) 0.0226(11) Uani 1 1 d . U . . .
C113 C 0.3219(3) -0.0278(3) 0.22750(14) 0.0223(10) Uani 1 1 d . U . . .
C114 C 0.3712(4) -0.0726(3) 0.20817(14) 0.0266(11) Uani 1 1 d . U . . .
H114 H 0.4366 -0.0462 0.2045 0.032 Uiso 1 1 calc R . . . .
C115 C 0.3220(4) -0.1569(3) 0.19438(15) 0.0318(12) Uani 1 1 d . U . . .
H115 H 0.3550 -0.1873 0.1821 0.038 Uiso 1 1 calc R . . . .
C116 C 0.2236(4) -0.1969(3) 0.19866(16) 0.0331(13) Uani 1 1 d . U . . .
H116 H 0.1912 -0.2534 0.1883 0.040 Uiso 1 1 calc R . . . .
C117 C 0.1733(4) -0.1531(3) 0.21831(15) 0.0289(12) Uani 1 1 d . U . . .
H117 H 0.1078 -0.1802 0.2216 0.035 Uiso 1 1 calc R . . . .
C118 C 0.2223(4) -0.0683(3) 0.23299(14) 0.0226(11) Uani 1 1 d . U . . .
C119 C 0.1897(4) -0.0062(3) 0.25393(14) 0.0243(11) Uani 1 1 d . U . . .
C120 C 0.1044(4) -0.0076(3) 0.26803(15) 0.0295(12) Uani 1 1 d . U . . .
H120 H 0.0493 -0.0569 0.2646 0.035 Uiso 1 1 calc R . . . .
C121 C 0.1015(4) 0.0681(4) 0.28801(16) 0.0349(13) Uani 1 1 d . U . . .
H121 H 0.0433 0.0674 0.2971 0.042 Uiso 1 1 calc R . . . .
C122 C 0.1812(4) 0.1416(3) 0.29430(15) 0.0326(13) Uani 1 1 d . U . . .
H122 H 0.1763 0.1896 0.3076 0.039 Uiso 1 1 calc R . . . .
C123 C 0.2722(4) 0.1457(3) 0.28059(14) 0.0262(11) Uani 1 1 d . U . . .
C124 C 0.3615(4) 0.2156(3) 0.28422(15) 0.0295(12) Uani 1 1 d . U . . .
H124 H 0.3658 0.2673 0.2970 0.035 Uiso 1 1 calc R . . . .
C125 C 0.4413(4) 0.2074(3) 0.26909(16) 0.0335(13) Uani 1 1 d . U . . .
H125 H 0.4995 0.2541 0.2722 0.040 Uiso 1 1 calc R . . . .
C126 C 0.4385(4) 0.1296(3) 0.24859(15) 0.0274(11) Uani 1 1 d . U . . .
H126 H 0.4935 0.1259 0.2378 0.033 Uiso 1 1 calc R . . . .
C127 C 0.3541(4) 0.0612(3) 0.24521(14) 0.0219(10) Uani 1 1 d . U . . .
C128 C 0.2718(3) 0.0704(3) 0.26114(14) 0.0207(10) Uani 1 1 d . U . . .
C129 C 0.7934(5) 0.5982(3) 0.02783(19) 0.0437(17) Uani 1 1 d . U . . .
C130 C 0.8174(6) 0.6774(4) 0.0524(2) 0.059(2) Uani 1 1 d . U . . .
H130 H 0.7765 0.7032 0.0504 0.071 Uiso 1 1 calc R . . . .
C131 C 0.9010(7) 0.7164(4) 0.0793(2) 0.067(2) Uani 1 1 d . U . . .
H131 H 0.9161 0.7689 0.0954 0.081 Uiso 1 1 calc R . . . .
C132 C 0.9645(6) 0.6805(4) 0.0833(2) 0.064(2) Uani 1 1 d . U . . .
H132 H 1.0210 0.7088 0.1019 0.077 Uiso 1 1 calc R . . . .
C133 C 0.9431(5) 0.6010(4) 0.05915(19) 0.0476(17) Uani 1 1 d . U . . .
H133 H 0.9850 0.5763 0.0615 0.057 Uiso 1 1 calc R . . . .
C134 C 0.8597(4) 0.5612(3) 0.03220(17) 0.0344(14) Uani 1 1 d . U . . .
C135 C 0.8165(4) 0.4794(3) 0.00247(16) 0.0254(12) Uani 1 1 d . U . . .
C136 C 0.8424(4) 0.4150(3) -0.00811(16) 0.0255(11) Uani 1 1 d . U . . .
H136 H 0.8993 0.4180 0.0049 0.031 Uiso 1 1 calc R . . . .
C137 C 0.7826(4) 0.3447(3) -0.03861(16) 0.0291(12) Uani 1 1 d . U . . .
H137 H 0.8014 0.3018 -0.0459 0.035 Uiso 1 1 calc R . . . .
C138 C 0.6968(4) 0.3369(3) -0.05819(17) 0.0294(12) Uani 1 1 d . U . . .
H138 H 0.6591 0.2895 -0.0784 0.035 Uiso 1 1 calc R . . . .
C139 C 0.6663(4) 0.4014(3) -0.04736(17) 0.0303(13) Uani 1 1 d . U . . .
C140 C 0.5800(4) 0.4042(4) -0.0635(2) 0.0438(16) Uani 1 1 d . U . . .
H140 H 0.5353 0.3599 -0.0835 0.053 Uiso 1 1 calc R . . . .
C141 C 0.5638(5) 0.4731(5) -0.0491(2) 0.055(2) Uani 1 1 d . U . . .
H141 H 0.5073 0.4739 -0.0599 0.067 Uiso 1 1 calc R . . . .
C142 C 0.6272(5) 0.5418(4) -0.0192(2) 0.0517(19) Uani 1 1 d . U . . .
H142 H 0.6127 0.5868 -0.0103 0.062 Uiso 1 1 calc R . . . .
C143 C 0.7123(5) 0.5419(4) -0.00293(19) 0.0406(16) Uani 1 1 d . U . . .
C144 C 0.7288(4) 0.4710(3) -0.01753(17) 0.0300(13) Uani 1 1 d . U . . .
C145 C 0.7043(3) 0.8901(3) 0.98925(13) 0.0191(10) Uani 1 1 d . U . . .
C146 C 0.6816(4) 0.8068(3) 0.98307(14) 0.0240(11) Uani 1 1 d . U . . .
H146 H 0.7265 0.7866 0.9736 0.029 Uiso 1 1 calc R . . . .
C147 C 0.5898(4) 0.7541(3) 0.99146(16) 0.0309(12) Uani 1 1 d . U . . .
H147 H 0.5734 0.6978 0.9875 0.037 Uiso 1 1 calc R . . . .
C148 C 0.5218(4) 0.7830(3) 1.00565(15) 0.0270(11) Uani 1 1 d . U . . .
H148 H 0.4606 0.7461 1.0107 0.032 Uiso 1 1 calc R . . . .
C149 C 0.5451(3) 0.8673(3) 1.01241(14) 0.0237(11) Uani 1 1 d . U . . .
H149 H 0.5002 0.8872 1.0223 0.028 Uiso 1 1 calc R . . . .
C150 C 0.6357(3) 0.9205(3) 1.00418(13) 0.0179(10) Uani 1 1 d . U . . .
C151 C 0.6813(3) 1.0117(3) 1.00833(13) 0.0165(9) Uani 1 1 d . U . . .
C152 C 0.6513(4) 1.0731(3) 1.01959(14) 0.0226(10) Uani 1 1 d . U . . .
H152 H 0.5891 1.0613 1.0278 0.027 Uiso 1 1 calc R . . . .
C153 C 0.7173(4) 1.1555(3) 1.01838(15) 0.0264(11) Uani 1 1 d . U . . .
H153 H 0.6974 1.1976 1.0262 0.032 Uiso 1 1 calc R . . . .
C154 C 0.8088(4) 1.1750(3) 1.00621(14) 0.0284(12) Uani 1 1 d . U . . .
H154 H 0.8500 1.2298 1.0062 0.034 Uiso 1 1 calc R . . . .
C155 C 0.8420(4) 1.1121(3) 0.99350(14) 0.0236(11) Uani 1 1 d . U . . .
C156 C 0.9330(4) 1.1203(3) 0.97808(14) 0.0279(12) Uani 1 1 d . U . . .
H156 H 0.9803 1.1721 0.9760 0.033 Uiso 1 1 calc R . . . .
C157 C 0.9500(4) 1.0520(3) 0.96647(15) 0.0270(11) Uani 1 1 d . U . . .
H157 H 1.0098 1.0589 0.9566 0.032 Uiso 1 1 calc R . . . .
C158 C 0.8818(3) 0.9710(3) 0.96850(14) 0.0235(11) Uani 1 1 d . U . . .
H158 H 0.8964 0.9259 0.9601 0.028 Uiso 1 1 calc R . . . .
C159 C 0.7937(3) 0.9608(3) 0.98323(13) 0.0188(10) Uani 1 1 d . U . . .
C160 C 0.7756(3) 1.0317(3) 0.99513(13) 0.0176(9) Uani 1 1 d . U . . .
C161 C 0.2097(3) 0.3953(3) 0.24416(14) 0.0202(10) Uani 1 1 d . U . . .
C162 C 0.1887(4) 0.3116(3) 0.23499(15) 0.0256(11) Uani 1 1 d . U . . .
H162 H 0.2350 0.2930 0.2411 0.031 Uiso 1 1 calc R . . . .
C163 C 0.0963(4) 0.2560(3) 0.21646(15) 0.0276(12) Uani 1 1 d . U . . .
H163 H 0.0814 0.1999 0.2105 0.033 Uiso 1 1 calc R . . . .
C164 C 0.0267(4) 0.2825(3) 0.20680(15) 0.0298(12) Uani 1 1 d . U . . .
H164 H -0.0339 0.2444 0.1942 0.036 Uiso 1 1 calc R . . . .
C165 C 0.0473(4) 0.3662(3) 0.21595(14) 0.0241(11) Uani 1 1 d . U . . .
H165 H 0.0008 0.3843 0.2095 0.029 Uiso 1 1 calc R . . . .
C166 C 0.1381(4) 0.4223(3) 0.23483(14) 0.0224(11) Uani 1 1 d . U . . .
C167 C 0.1808(4) 0.5132(3) 0.24841(14) 0.0233(11) Uani 1 1 d . U . . .
C168 C 0.1482(4) 0.5742(3) 0.24911(14) 0.0250(11) Uani 1 1 d . U . . .
H168 H 0.0854 0.5614 0.2387 0.030 Uiso 1 1 calc R . . . .
C169 C 0.2130(4) 0.6562(3) 0.26603(15) 0.0260(11) Uani 1 1 d . U . . .
H169 H 0.1911 0.6973 0.2667 0.031 Uiso 1 1 calc R . . . .
C170 C 0.3063(4) 0.6789(3) 0.28149(15) 0.0272(12) Uani 1 1 d . U . . .
H170 H 0.3463 0.7342 0.2920 0.033 Uiso 1 1 calc R . . . .
C171 C 0.3420(4) 0.6178(3) 0.28136(14) 0.0244(11) Uani 1 1 d . U . . .
C172 C 0.4345(4) 0.6286(3) 0.29750(15) 0.0263(11) Uani 1 1 d . U . . .
H172 H 0.4811 0.6813 0.3089 0.032 Uiso 1 1 calc R . . . .
C173 C 0.4554(4) 0.5610(3) 0.29631(15) 0.0269(11) Uani 1 1 d . U . . .
H173 H 0.5163 0.5696 0.3073 0.032 Uiso 1 1 calc R . . . .
C174 C 0.3885(4) 0.4796(3) 0.27912(15) 0.0256(11) Uani 1 1 d . U . . .
H174 H 0.4049 0.4354 0.2786 0.031 Uiso 1 1 calc R . . . .
C175 C 0.2991(4) 0.4676(3) 0.26336(14) 0.0211(10) Uani 1 1 d . U . . .
C176 C 0.2772(3) 0.5362(3) 0.26482(14) 0.0196(10) Uani 1 1 d . U . . .
F1 F 0.8439(2) 0.93314(18) 0.32756(9) 0.0320(7) Uani 1 1 d . . . . .
F2 F 0.6664(2) 0.80981(16) 0.31686(9) 0.0327(7) Uani 1 1 d . . . . .
F3 F 0.5152(2) 0.83652(16) 0.34980(9) 0.0314(7) Uani 1 1 d . . . . .
F4 F 0.54319(19) 0.98344(17) 0.39716(9) 0.0290(7) Uani 1 1 d . . . . .
F5 F 0.5035(2) 0.10338(19) 0.35233(9) 0.0377(8) Uani 1 1 d . . . . .
F6 F 0.4101(2) -0.05730(19) 0.31841(9) 0.0411(8) Uani 1 1 d . . . . .
F7 F 0.2196(2) -0.13819(18) 0.32655(9) 0.0435(8) Uani 1 1 d . . . . .
F8 F 0.1216(2) -0.05885(18) 0.36989(9) 0.0371(8) Uani 1 1 d . . . . .
F9 F 0.0355(2) 0.44186(18) 0.08328(9) 0.0342(7) Uani 1 1 d . . . . .
F10 F 0.1284(2) 0.59602(17) 0.12883(9) 0.0344(7) Uani 1 1 d . . . . .
F11 F 0.3066(2) 0.64705(16) 0.16965(9) 0.0337(7) Uani 1 1 d . . . . .
F12 F 0.3891(2) 0.54205(17) 0.16834(8) 0.0298(7) Uani 1 1 d . . . . .
F13 F 0.0410(2) 0.48562(18) 0.34094(8) 0.0316(7) Uani 1 1 d . . . . .
F14 F 0.1646(2) 0.64374(17) 0.36505(9) 0.0304(7) Uani 1 1 d . . . . .
F15 F 0.3500(2) 0.68367(16) 0.39272(8) 0.0301(7) Uani 1 1 d . . . . .
F16 F 0.40763(19) 0.56531(16) 0.40255(8) 0.0261(6) Uani 1 1 d . . . . .
F17 F 0.6908(3) 0.5809(2) 0.13124(11) 0.0656(13) Uani 1 1 d . . . . .
F18 F 0.8567(3) 0.6851(2) 0.17921(11) 0.0702(14) Uani 1 1 d . . . . .
F19 F 0.9939(2) 0.63444(18) 0.19632(9) 0.0487(9) Uani 1 1 d . . . . .
F20 F 0.9648(2) 0.47819(18) 0.16861(9) 0.0312(7) Uani 1 1 d . . . . .
F21 F 0.7160(2) 0.63502(17) 0.37452(9) 0.0296(7) Uani 1 1 d . . . . .
F22 F 0.9005(2) 0.72468(16) 0.40665(9) 0.0310(7) Uani 1 1 d . . . . .
F23 F 1.0133(2) 0.64950(18) 0.42527(9) 0.0320(7) Uani 1 1 d . . . . .
F24 F 0.9406(2) 0.48516(17) 0.41577(9) 0.0304(7) Uani 1 1 d . . . . .
F25 F 0.5392(2) 0.95511(19) 0.14726(9) 0.0343(7) Uani 1 1 d . . . . .
F26 F 0.5115(2) 0.79912(18) 0.11941(9) 0.0344(7) Uani 1 1 d . . . . .
F27 F 0.6599(2) 0.76363(16) 0.08996(9) 0.0306(7) Uani 1 1 d . . . . .
F28 F 0.8320(2) 0.88540(17) 0.08355(8) 0.0288(7) Uani 1 1 d . . . . .
F29 F 0.4772(2) 1.02634(18) 0.08723(9) 0.0319(7) Uani 1 1 d . . . . .
F30 F 0.3599(2) 0.86674(17) 0.08141(8) 0.0306(7) Uani 1 1 d . . . . .
F31 F 0.1753(2) 0.82083(16) 0.10313(9) 0.0315(7) Uani 1 1 d . . . . .
F32 F 0.1124(2) 0.93479(17) 0.13656(8) 0.0306(7) Uani 1 1 d . . . . .
I1 I 0.72420(3) 1.15012(2) 0.42473(2) 0.02859(8) Uani 1 1 d . . . . .
I2 I 0.92798(2) 1.11538(2) 0.37768(2) 0.02981(8) Uani 1 1 d . . . . .
I3 I 0.18401(3) 0.12310(2) 0.42006(2) 0.03448(9) Uani 1 1 d . . . . .
I4 I 0.44185(3) 0.23213(2) 0.40683(2) 0.03719(9) Uani 1 1 d . . . . .
I5 I 0.32406(3) 0.35594(2) 0.12562(2) 0.02868(8) Uani 1 1 d . . . . .
I6 I 0.08212(3) 0.28776(2) 0.06892(2) 0.03161(8) Uani 1 1 d . . . . .
I7 I 0.30352(2) 0.37233(2) 0.38471(2) 0.02655(8) Uani 1 1 d . . . . .
I8 I 0.05246(2) 0.31922(2) 0.34484(2) 0.03080(8) Uani 1 1 d . . . . .
I9 I 0.79836(3) 0.32619(2) 0.11189(2) 0.03552(9) Uani 1 1 d . . . . .
I10 I 0.61233(3) 0.39516(3) 0.08531(2) 0.05390(13) Uani 1 1 d . . . . .
I11 I 0.74154(3) 0.34398(2) 0.37940(2) 0.03320(9) Uani 1 1 d . . . . .
I12 I 0.58524(3) 0.44574(2) 0.35474(2) 0.03431(9) Uani 1 1 d . . . . .
I13 I 0.71471(3) 1.12475(2) 0.15081(2) 0.03235(8) Uani 1 1 d . . . . .
I14 I 0.91506(2) 1.07771(2) 0.10904(2) 0.03080(8) Uani 1 1 d . . . . .
I15 I 0.20794(3) 1.12751(2) 0.15504(2) 0.03133(8) Uani 1 1 d . . . . .
I16 I 0.45803(3) 1.18916(2) 0.12252(2) 0.03086(8) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.023(3) 0.020(2) 0.012(2) 0.0041(18) -0.0053(18) 0.007(2)
C2 0.013(2) 0.019(2) 0.018(2) 0.0095(19) -0.0022(17) -0.0012(18)
C3 0.024(3) 0.025(2) 0.014(2) 0.0080(19) 0.0021(18) 0.011(2)
C4 0.032(3) 0.017(2) 0.012(2) 0.0009(18) -0.0036(19) 0.009(2)
C5 0.020(3) 0.024(3) 0.022(2) 0.009(2) -0.0066(19) 0.001(2)
C6 0.019(3) 0.028(3) 0.017(2) 0.010(2) -0.0016(18) 0.010(2)
C7 0.022(3) 0.023(2) 0.011(2) 0.0036(18) -0.0014(17) 0.010(2)
C8 0.018(3) 0.028(3) 0.020(2) 0.012(2) -0.0047(19) 0.004(2)
C9 0.019(3) 0.041(3) 0.021(2) 0.014(2) 0.002(2) 0.015(2)
C10 0.039(3) 0.036(3) 0.017(2) 0.006(2) 0.000(2) 0.025(3)
C11 0.040(3) 0.025(3) 0.016(2) 0.007(2) -0.005(2) 0.009(2)
C12 0.020(3) 0.031(3) 0.018(2) 0.011(2) -0.0039(19) -0.001(2)
C13 0.027(3) 0.021(2) 0.015(2) 0.0049(19) 0.0083(19) 0.010(2)
C14 0.021(3) 0.019(2) 0.014(2) 0.0011(18) 0.0055(19) 0.001(2)
C15 0.020(3) 0.025(3) 0.016(2) 0.0026(19) 0.0058(19) 0.006(2)
C16 0.030(3) 0.024(3) 0.023(2) 0.005(2) 0.011(2) 0.016(2)
C17 0.035(3) 0.025(3) 0.014(2) 0.003(2) 0.011(2) 0.011(2)
C18 0.019(3) 0.026(3) 0.013(2) 0.0027(19) 0.0017(18) 0.004(2)
C19 0.030(3) 0.021(2) 0.0075(19) 0.0033(18) 0.0057(18) 0.009(2)
C20 0.020(3) 0.021(2) 0.015(2) 0.0022(19) 0.0032(19) 0.000(2)
C21 0.015(3) 0.035(3) 0.011(2) 0.002(2) 0.0042(18) 0.005(2)
C22 0.026(3) 0.025(3) 0.013(2) -0.0006(19) 0.0027(19) 0.012(2)
C23 0.029(3) 0.020(2) 0.014(2) 0.0015(19) 0.0067(19) 0.007(2)
C24 0.014(2) 0.027(3) 0.011(2) 0.0011(19) 0.0007(17) 0.002(2)
C25 0.029(3) 0.018(2) 0.014(2) 0.0064(18) 0.0110(19) 0.010(2)
C26 0.033(3) 0.038(3) 0.021(2) 0.019(2) 0.011(2) 0.019(2)
C27 0.056(4) 0.057(4) 0.032(3) 0.030(3) 0.027(3) 0.045(3)
C28 0.068(4) 0.026(3) 0.027(3) 0.012(2) 0.027(3) 0.026(3)
C29 0.043(3) 0.019(3) 0.018(2) 0.002(2) 0.010(2) 0.005(2)
C30 0.024(3) 0.023(2) 0.015(2) 0.0075(19) 0.0080(19) 0.005(2)
C31 0.029(3) 0.018(2) 0.013(2) 0.0041(18) 0.0058(19) 0.008(2)
C32 0.017(2) 0.025(2) 0.015(2) 0.0059(19) 0.0039(18) 0.005(2)
C33 0.030(3) 0.024(3) 0.015(2) 0.0021(19) 0.007(2) 0.018(2)
C34 0.026(3) 0.018(2) 0.018(2) 0.0057(19) 0.008(2) 0.008(2)
C35 0.020(3) 0.032(3) 0.018(2) 0.005(2) 0.005(2) 0.005(2)
C36 0.037(3) 0.031(3) 0.013(2) 0.009(2) 0.011(2) 0.022(2)
C37 0.027(3) 0.017(2) 0.014(2) 0.0043(18) -0.0024(18) 0.009(2)
C38 0.024(3) 0.021(2) 0.012(2) 0.0049(18) 0.0008(18) 0.005(2)
C39 0.025(3) 0.025(3) 0.016(2) 0.0032(19) -0.0008(19) 0.010(2)
C40 0.029(3) 0.020(2) 0.018(2) 0.0056(19) -0.001(2) 0.008(2)
C41 0.023(3) 0.033(3) 0.016(2) 0.014(2) 0.0015(19) 0.009(2)
C42 0.024(3) 0.036(3) 0.014(2) 0.012(2) 0.0065(19) 0.017(2)
C43 0.026(3) 0.025(2) 0.011(2) 0.0010(18) -0.0041(18) 0.012(2)
C44 0.031(3) 0.024(2) 0.010(2) 0.0049(19) -0.0020(19) 0.010(2)
C45 0.027(3) 0.028(3) 0.013(2) 0.0091(19) 0.0041(19) 0.014(2)
C46 0.031(3) 0.032(3) 0.014(2) 0.006(2) 0.0001(19) 0.019(2)
C47 0.027(3) 0.024(3) 0.011(2) 0.0018(19) -0.0076(18) 0.006(2)
C48 0.020(3) 0.032(3) 0.017(2) 0.007(2) 0.0024(19) 0.009(2)
C49 0.028(3) 0.030(3) 0.022(2) 0.017(2) 0.007(2) 0.013(2)
C50 0.044(3) 0.047(3) 0.028(3) 0.024(3) 0.013(2) 0.024(3)
C51 0.072(4) 0.045(4) 0.029(3) 0.017(3) 0.014(3) 0.039(3)
C52 0.074(4) 0.026(3) 0.027(3) 0.011(2) -0.001(3) 0.019(3)
C53 0.043(3) 0.023(3) 0.026(3) 0.015(2) -0.002(2) 0.003(2)
C54 0.032(3) 0.023(3) 0.021(2) 0.014(2) 0.002(2) 0.008(2)
C55 0.021(3) 0.028(3) 0.021(2) 0.015(2) -0.0016(19) 0.008(2)
C56 0.018(3) 0.040(3) 0.033(3) 0.018(2) -0.001(2) 0.009(2)
C57 0.033(3) 0.059(4) 0.034(3) 0.022(3) 0.006(2) 0.032(3)
C58 0.051(4) 0.035(3) 0.029(3) 0.011(2) 0.000(2) 0.030(3)
C59 0.039(3) 0.029(3) 0.026(3) 0.014(2) -0.002(2) 0.018(2)
C60 0.054(4) 0.022(3) 0.029(3) 0.011(2) -0.014(3) 0.007(3)
C61 0.037(3) 0.031(3) 0.034(3) 0.018(2) -0.013(2) -0.002(2)
C62 0.022(3) 0.040(3) 0.044(3) 0.026(3) -0.001(2) 0.005(2)
C63 0.021(3) 0.029(3) 0.029(3) 0.019(2) 0.000(2) 0.007(2)
C64 0.021(3) 0.025(3) 0.022(2) 0.015(2) -0.0024(19) 0.007(2)
C65 0.023(3) 0.021(2) 0.0084(19) 0.0049(18) 0.0030(18) 0.008(2)
C66 0.022(3) 0.032(3) 0.011(2) 0.0037(19) 0.0013(18) 0.012(2)
C67 0.044(3) 0.032(3) 0.017(2) 0.005(2) 0.004(2) 0.022(3)
C68 0.034(3) 0.017(2) 0.020(2) 0.0017(19) 0.008(2) 0.005(2)
C69 0.019(3) 0.030(3) 0.014(2) 0.000(2) 0.0023(18) 0.004(2)
C70 0.017(2) 0.022(2) 0.0084(19) 0.0010(17) 0.0040(17) 0.0039(19)
C71 0.014(2) 0.028(2) 0.0093(19) 0.0023(18) 0.0040(17) 0.008(2)
C72 0.022(3) 0.036(3) 0.018(2) 0.004(2) 0.0060(19) 0.013(2)
C73 0.036(3) 0.049(3) 0.018(2) 0.005(2) 0.003(2) 0.027(3)
C74 0.040(3) 0.032(3) 0.022(2) 0.009(2) 0.008(2) 0.022(3)
C75 0.031(3) 0.025(3) 0.015(2) 0.0047(19) 0.009(2) 0.012(2)
C76 0.041(3) 0.021(3) 0.021(2) 0.003(2) 0.014(2) 0.008(2)
C77 0.025(3) 0.023(3) 0.020(2) -0.001(2) 0.007(2) -0.004(2)
C78 0.021(3) 0.021(2) 0.016(2) -0.0009(19) 0.0038(19) 0.005(2)
C79 0.018(2) 0.020(2) 0.0092(19) 0.0020(17) 0.0055(17) 0.0043(19)
C80 0.020(3) 0.023(2) 0.011(2) 0.0060(18) 0.0070(18) 0.008(2)
C81 0.022(3) 0.022(2) 0.0106(19) 0.0054(18) 0.0003(17) 0.009(2)
C82 0.023(3) 0.031(3) 0.016(2) 0.003(2) -0.0007(19) 0.012(2)
C83 0.044(4) 0.034(3) 0.025(3) 0.005(2) -0.006(2) 0.023(3)
C84 0.042(3) 0.025(3) 0.028(3) 0.009(2) -0.013(2) 0.005(2)
C85 0.023(3) 0.046(3) 0.027(3) 0.021(3) -0.003(2) 0.003(2)
C86 0.024(3) 0.033(3) 0.016(2) 0.011(2) 0.0019(19) 0.013(2)
C87 0.042(3) 0.067(4) 0.015(2) 0.013(2) 0.003(2) 0.039(3)
C88 0.049(4) 0.120(6) 0.029(3) 0.021(3) 0.006(3) 0.061(4)
C89 0.098(6) 0.150(7) 0.035(3) 0.017(4) 0.000(4) 0.102(5)
C90 0.134(7) 0.105(6) 0.037(3) 0.005(4) -0.002(4) 0.109(5)
C91 0.105(5) 0.063(4) 0.027(3) 0.009(3) -0.005(3) 0.065(4)
C92 0.142(7) 0.041(4) 0.027(3) 0.003(3) -0.018(4) 0.053(4)
C93 0.103(5) 0.030(3) 0.027(3) 0.014(3) -0.020(3) 0.006(3)
C94 0.056(4) 0.024(3) 0.023(3) 0.008(2) -0.011(2) 0.003(3)
C95 0.038(3) 0.026(3) 0.011(2) 0.0077(19) -0.0026(19) 0.016(2)
C96 0.053(4) 0.044(3) 0.017(2) 0.007(2) -0.002(2) 0.037(3)
C97 0.039(3) 0.028(3) 0.016(2) 0.004(2) 0.013(2) 0.005(2)
C98 0.055(4) 0.044(3) 0.026(3) 0.009(3) 0.013(3) 0.014(3)
C99 0.056(4) 0.038(3) 0.034(3) 0.002(3) 0.009(3) -0.007(3)
C100 0.039(4) 0.065(4) 0.029(3) 0.004(3) 0.009(3) -0.010(3)
C101 0.030(3) 0.060(4) 0.025(3) 0.007(3) 0.006(2) 0.010(3)
C102 0.021(3) 0.050(3) 0.014(2) 0.008(2) 0.007(2) 0.010(2)
C103 0.025(3) 0.042(3) 0.016(2) 0.008(2) 0.004(2) 0.017(2)
C104 0.032(3) 0.058(4) 0.022(2) 0.013(3) 0.006(2) 0.025(3)
C105 0.054(4) 0.035(3) 0.026(3) 0.010(2) 0.008(3) 0.025(3)
C106 0.048(4) 0.031(3) 0.024(3) 0.009(2) 0.012(3) 0.012(3)
C107 0.035(3) 0.040(3) 0.017(2) 0.006(2) 0.008(2) 0.015(3)
C108 0.021(3) 0.041(3) 0.023(2) 0.002(2) 0.004(2) 0.008(2)
C109 0.024(3) 0.059(4) 0.024(3) 0.008(3) 0.008(2) 0.019(3)
C110 0.042(3) 0.048(3) 0.022(2) 0.012(2) 0.012(2) 0.028(3)
C111 0.025(3) 0.042(3) 0.018(2) 0.013(2) 0.011(2) 0.018(2)
C112 0.024(3) 0.030(3) 0.014(2) 0.006(2) 0.0090(19) 0.011(2)
C113 0.025(3) 0.030(3) 0.012(2) 0.0048(19) -0.0023(18) 0.011(2)
C114 0.032(3) 0.037(3) 0.015(2) 0.007(2) 0.005(2) 0.018(2)
C115 0.052(4) 0.035(3) 0.017(2) 0.004(2) 0.001(2) 0.028(3)
C116 0.049(4) 0.026(3) 0.025(3) 0.007(2) -0.004(2) 0.016(3)
C117 0.031(3) 0.032(3) 0.021(2) 0.011(2) -0.003(2) 0.008(2)
C118 0.030(3) 0.028(3) 0.010(2) 0.0067(19) -0.0017(19) 0.011(2)
C119 0.032(3) 0.033(3) 0.013(2) 0.008(2) -0.0002(19) 0.017(2)
C120 0.027(3) 0.039(3) 0.023(2) 0.007(2) 0.003(2) 0.015(2)
C121 0.032(3) 0.061(4) 0.024(3) 0.009(3) 0.004(2) 0.031(3)
C122 0.049(4) 0.039(3) 0.019(2) 0.000(2) -0.001(2) 0.029(3)
C123 0.035(3) 0.035(3) 0.013(2) 0.004(2) -0.003(2) 0.019(2)
C124 0.047(3) 0.025(3) 0.019(2) 0.003(2) -0.002(2) 0.018(2)
C125 0.035(3) 0.033(3) 0.024(3) 0.005(2) -0.003(2) 0.007(2)
C126 0.027(3) 0.030(3) 0.025(2) 0.008(2) 0.003(2) 0.012(2)
C127 0.030(3) 0.028(3) 0.010(2) 0.0065(19) 0.0016(19) 0.013(2)
C128 0.026(3) 0.026(3) 0.012(2) 0.0053(19) -0.0017(18) 0.013(2)
C129 0.069(4) 0.028(3) 0.044(3) 0.021(3) 0.044(3) 0.025(3)
C130 0.105(6) 0.031(3) 0.053(4) 0.024(3) 0.058(4) 0.032(4)
C131 0.112(6) 0.028(3) 0.046(4) 0.010(3) 0.053(4) 0.012(4)
C132 0.072(5) 0.047(4) 0.045(4) 0.009(3) 0.035(4) -0.003(3)
C133 0.049(4) 0.036(3) 0.040(3) 0.005(3) 0.025(3) 0.001(3)
C134 0.048(4) 0.023(3) 0.032(3) 0.014(2) 0.030(3) 0.011(3)
C135 0.032(3) 0.023(3) 0.027(2) 0.013(2) 0.020(2) 0.014(2)
C136 0.025(3) 0.028(3) 0.028(3) 0.012(2) 0.010(2) 0.013(2)
C137 0.041(3) 0.025(3) 0.031(3) 0.013(2) 0.015(2) 0.020(2)
C138 0.035(3) 0.022(3) 0.033(3) 0.014(2) 0.013(2) 0.011(2)
C139 0.028(3) 0.039(3) 0.033(3) 0.027(3) 0.021(2) 0.016(2)
C140 0.036(3) 0.056(4) 0.051(3) 0.037(3) 0.023(3) 0.020(3)
C141 0.053(4) 0.077(5) 0.073(4) 0.059(4) 0.040(4) 0.048(4)
C142 0.073(5) 0.054(4) 0.064(4) 0.041(3) 0.053(4) 0.049(4)
C143 0.059(4) 0.039(3) 0.047(3) 0.032(3) 0.039(3) 0.033(3)
C144 0.035(3) 0.029(3) 0.037(3) 0.022(2) 0.026(3) 0.018(2)
C145 0.025(3) 0.025(2) 0.011(2) 0.0057(18) 0.0026(18) 0.013(2)
C146 0.034(3) 0.025(3) 0.019(2) 0.005(2) 0.000(2) 0.019(2)
C147 0.040(3) 0.025(3) 0.027(3) 0.009(2) -0.004(2) 0.012(2)
C148 0.023(3) 0.030(3) 0.023(2) 0.013(2) 0.001(2) 0.003(2)
C149 0.021(3) 0.035(3) 0.018(2) 0.009(2) 0.0045(19) 0.014(2)
C150 0.024(3) 0.024(2) 0.0097(19) 0.0035(18) 0.0015(18) 0.014(2)
C151 0.021(3) 0.021(2) 0.0090(19) 0.0029(17) -0.0013(17) 0.0093(19)
C152 0.027(3) 0.028(3) 0.014(2) 0.0029(19) 0.0003(19) 0.013(2)
C153 0.041(3) 0.020(2) 0.021(2) 0.003(2) -0.004(2) 0.017(2)
C154 0.036(3) 0.025(3) 0.016(2) 0.003(2) -0.008(2) 0.005(2)
C155 0.028(3) 0.027(3) 0.012(2) 0.0066(19) -0.0014(19) 0.007(2)
C156 0.026(3) 0.033(3) 0.015(2) 0.011(2) -0.0014(19) 0.000(2)
C157 0.015(3) 0.044(3) 0.018(2) 0.006(2) -0.0028(19) 0.008(2)
C158 0.022(3) 0.036(3) 0.016(2) 0.002(2) -0.0005(19) 0.018(2)
C159 0.025(3) 0.025(2) 0.0095(19) 0.0008(18) -0.0028(18) 0.014(2)
C160 0.019(2) 0.029(3) 0.0082(19) 0.0053(18) -0.0033(17) 0.012(2)
C161 0.028(3) 0.020(2) 0.013(2) 0.0050(18) 0.0088(19) 0.009(2)
C162 0.030(3) 0.029(3) 0.018(2) 0.004(2) 0.009(2) 0.013(2)
C163 0.033(3) 0.020(3) 0.023(2) -0.001(2) 0.008(2) 0.006(2)
C164 0.031(3) 0.023(3) 0.024(2) 0.001(2) 0.004(2) 0.003(2)
C165 0.021(3) 0.029(3) 0.018(2) 0.004(2) 0.0027(19) 0.008(2)
C166 0.031(3) 0.024(3) 0.011(2) 0.0061(19) 0.0071(19) 0.010(2)
C167 0.032(3) 0.027(3) 0.011(2) 0.0070(19) 0.009(2) 0.011(2)
C168 0.029(3) 0.031(3) 0.017(2) 0.007(2) 0.003(2) 0.014(2)
C169 0.038(3) 0.024(3) 0.020(2) 0.008(2) 0.005(2) 0.015(2)
C170 0.032(3) 0.024(3) 0.018(2) 0.003(2) 0.005(2) 0.003(2)
C171 0.029(3) 0.027(3) 0.015(2) 0.008(2) 0.010(2) 0.008(2)
C172 0.029(3) 0.025(3) 0.020(2) 0.007(2) 0.009(2) 0.005(2)
C173 0.022(3) 0.036(3) 0.022(2) 0.007(2) 0.006(2) 0.010(2)
C174 0.028(3) 0.028(3) 0.025(2) 0.011(2) 0.011(2) 0.014(2)
C175 0.026(3) 0.022(2) 0.014(2) 0.0038(19) 0.0061(19) 0.009(2)
C176 0.023(3) 0.022(2) 0.010(2) 0.0056(18) 0.0047(18) 0.005(2)
F1 0.0332(18) 0.0421(18) 0.0251(15) 0.0041(13) 0.0052(13) 0.0210(15)
F2 0.048(2) 0.0234(16) 0.0241(14) -0.0023(12) -0.0078(13) 0.0144(14)
F3 0.0205(16) 0.0258(16) 0.0367(16) 0.0105(13) -0.0075(12) -0.0030(13)
F4 0.0206(16) 0.0381(17) 0.0318(15) 0.0114(14) 0.0058(12) 0.0138(14)
F5 0.0236(18) 0.058(2) 0.0343(17) 0.0175(16) 0.0054(14) 0.0164(16)
F6 0.057(2) 0.053(2) 0.0294(16) 0.0054(15) 0.0018(15) 0.0395(19)
F7 0.065(2) 0.0228(17) 0.0268(16) -0.0008(13) -0.0097(15) 0.0047(16)
F8 0.0223(17) 0.0421(19) 0.0311(16) 0.0117(14) -0.0057(13) -0.0039(14)
F9 0.0208(17) 0.0449(19) 0.0356(16) 0.0054(15) 0.0030(13) 0.0130(15)
F10 0.0391(19) 0.0371(18) 0.0384(17) 0.0109(14) 0.0160(15) 0.0255(16)
F11 0.0401(19) 0.0187(15) 0.0304(16) -0.0056(12) 0.0056(14) 0.0042(14)
F12 0.0256(17) 0.0317(16) 0.0238(14) 0.0003(13) -0.0032(12) 0.0057(13)
F13 0.0193(16) 0.0473(19) 0.0219(14) 0.0063(14) 0.0010(12) 0.0076(14)
F14 0.0364(18) 0.0309(17) 0.0257(15) 0.0037(13) 0.0041(13) 0.0165(14)
F15 0.0350(18) 0.0206(15) 0.0220(14) -0.0024(12) -0.0020(12) 0.0016(13)
F16 0.0150(15) 0.0321(16) 0.0230(14) 0.0021(12) -0.0039(11) 0.0030(12)
F17 0.093(3) 0.112(3) 0.055(2) 0.057(2) 0.046(2) 0.089(3)
F18 0.161(4) 0.034(2) 0.039(2) 0.0157(17) 0.042(2) 0.060(3)
F19 0.061(2) 0.0280(18) 0.0258(16) -0.0050(14) 0.0076(16) -0.0090(16)
F20 0.0263(17) 0.0434(18) 0.0255(15) 0.0084(14) 0.0033(13) 0.0156(15)
F21 0.0332(18) 0.0366(17) 0.0283(15) 0.0122(13) 0.0063(13) 0.0214(15)
F22 0.0386(19) 0.0194(15) 0.0311(15) 0.0072(13) 0.0067(13) 0.0073(13)
F23 0.0217(17) 0.0392(18) 0.0282(15) 0.0068(14) 0.0026(12) 0.0057(14)
F24 0.0370(18) 0.0423(18) 0.0254(15) 0.0107(14) 0.0099(13) 0.0283(15)
F25 0.0293(18) 0.056(2) 0.0303(16) 0.0173(15) 0.0097(13) 0.0274(16)
F26 0.0198(16) 0.0399(18) 0.0362(17) 0.0196(15) 0.0043(13) 0.0008(14)
F27 0.0376(19) 0.0218(15) 0.0288(15) 0.0064(13) -0.0012(13) 0.0083(14)
F28 0.0269(17) 0.0367(17) 0.0259(14) 0.0038(13) 0.0050(12) 0.0171(14)
F29 0.0239(17) 0.0486(19) 0.0285(15) 0.0150(14) 0.0074(13) 0.0175(15)
F30 0.044(2) 0.0344(17) 0.0242(14) 0.0013(13) 0.0027(13) 0.0290(15)
F31 0.0378(19) 0.0225(15) 0.0260(15) 0.0037(12) -0.0038(13) 0.0049(14)
F32 0.0252(17) 0.0424(18) 0.0241(14) 0.0081(13) 0.0054(12) 0.0133(14)
I1 0.0435(2) 0.02282(17) 0.02096(15) 0.00051(13) -0.00436(14) 0.01675(16)
I2 0.01965(18) 0.03399(19) 0.02488(16) 0.01135(15) -0.00178(13) -0.00159(14)
I3 0.0377(2) 0.0555(2) 0.02214(16) 0.01250(16) 0.00792(15) 0.02923(19)
I4 0.0386(2) 0.02649(19) 0.03049(18) 0.00458(15) -0.01040(15) -0.00170(16)
I5 0.0354(2) 0.03197(19) 0.02438(16) 0.00786(14) 0.00553(14) 0.01869(16)
I6 0.0321(2) 0.02371(17) 0.02545(16) -0.00048(14) 0.00135(14) 0.00015(15)
I7 0.0350(2) 0.02722(18) 0.01904(15) 0.00525(13) 0.00666(14) 0.01415(15)
I8 0.02736(19) 0.02604(18) 0.02061(15) 0.00039(13) 0.00273(13) -0.00551(14)
I9 0.0518(2) 0.01825(17) 0.03105(18) 0.00173(14) 0.01228(17) 0.01021(16)
I10 0.0228(2) 0.0986(4) 0.0332(2) 0.0368(2) 0.00397(16) 0.0094(2)
I11 0.0537(2) 0.02075(17) 0.02382(16) 0.00360(14) 0.01108(16) 0.01434(16)
I12 0.0251(2) 0.0419(2) 0.02683(17) 0.00855(16) -0.00328(14) 0.00433(16)
I13 0.0497(2) 0.03209(19) 0.02165(16) 0.00308(14) -0.00380(15) 0.02420(18)
I14 0.02430(19) 0.03243(19) 0.02297(16) 0.00371(14) 0.00006(13) -0.00008(15)
I15 0.0453(2) 0.0401(2) 0.01881(15) 0.00061(14) 0.00009(14) 0.02962(18)
I16 0.0352(2) 0.02594(18) 0.02537(16) 0.00949(14) -0.00498(14) 0.00526(15)
_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
C1 C2 1.406(6) . ?
C1 C6 1.374(6) . ?
C1 I1 2.086(4) . ?
C2 C3 1.379(6) . ?
C2 I2 2.078(4) . ?
C3 C4 1.367(6) . ?
C3 F1 1.352(5) . ?
C4 C5 1.381(6) . ?
C4 F2 1.334(5) . ?
C5 C6 1.384(7) . ?
C5 F3 1.338(5) . ?
C6 F4 1.346(5) . ?
C7 C8 1.398(6) . ?
C7 C12 1.387(6) . ?
C7 I3 2.079(4) . ?
C8 C9 1.383(7) . ?
C8 I4 2.081(5) . ?
C9 C10 1.368(7) . ?
C9 F5 1.351(5) . ?
C10 C11 1.372(7) . ?
C10 F6 1.340(5) . ?
C11 C12 1.383(7) . ?
C11 F7 1.333(6) . ?
C12 F8 1.340(5) . ?
C13 C14 1.398(7) . ?
C13 C18 1.378(6) . ?
C13 I5 2.085(5) . ?
C14 C15 1.382(6) . ?
C14 I6 2.084(5) . ?
C15 C16 1.381(7) . ?
C15 F9 1.352(6) . ?
C16 C17 1.366(7) . ?
C16 F10 1.341(5) . ?
C17 C18 1.379(7) . ?
C17 F11 1.344(5) . ?
C18 F12 1.351(5) . ?
C19 C20 1.395(7) . ?
C19 C24 1.377(6) . ?
C19 I7 2.097(5) . ?
C20 C21 1.371(7) . ?
C20 I8 2.088(5) . ?
C21 C22 1.376(7) . ?
C21 F13 1.343(5) . ?
C22 C23 1.366(7) . ?
C22 F14 1.346(5) . ?
C23 C24 1.385(6) . ?
C23 F15 1.339(5) . ?
C24 F16 1.346(5) . ?
C25 C26 1.400(6) . ?
C25 C30 1.392(7) . ?
C25 I9 2.073(4) . ?
C26 C27 1.387(7) . ?
C26 I10 2.086(6) . ?
C27 C28 1.372(9) . ?
C27 F17 1.346(6) . ?
C28 C29 1.365(8) . ?
C28 F18 1.325(6) . ?
C29 C30 1.370(6) . ?
C29 F19 1.341(6) . ?
C30 F20 1.340(5) . ?
C31 C32 1.387(6) . ?
C31 C36 1.383(7) . ?
C31 I11 2.084(4) . ?
C32 C33 1.377(6) . ?
C32 I12 2.083(5) . ?
C33 C34 1.369(7) . ?
C33 F21 1.349(5) . ?
C34 C35 1.383(7) . ?
C34 F22 1.345(5) . ?
C35 C36 1.380(7) . ?
C35 F23 1.336(6) . ?
C36 F24 1.353(5) . ?
C37 C38 1.415(6) . ?
C37 C42 1.378(6) . ?
C37 I13 2.078(4) . ?
C38 C39 1.376(6) . ?
C38 I14 2.087(4) . ?
C39 C40 1.385(6) . ?
C39 F28 1.345(5) . ?
C40 C41 1.375(6) . ?
C40 F27 1.335(5) . ?
C41 C42 1.366(7) . ?
C41 F26 1.344(5) . ?
C42 F25 1.345(5) . ?
C43 C44 1.392(6) . ?
C43 C48 1.374(6) . ?
C43 I15 2.088(4) . ?
C44 C45 1.396(6) . ?
C44 I16 2.085(5) . ?
C45 C46 1.358(6) . ?
C45 F29 1.356(5) . ?
C46 C47 1.377(6) . ?
C46 F30 1.335(5) . ?
C47 C48 1.377(6) . ?
C47 F31 1.339(5) . ?
C48 F32 1.351(5) . ?
C49 C50 1.389(7) . ?
C49 C54 1.424(7) . ?
C49 C63 1.468(7) . ?
C50 H50 0.9300 . ?
C50 C51 1.385(8) . ?
C51 H51 0.9300 . ?
C51 C52 1.365(8) . ?
C52 H52 0.9300 . ?
C52 C53 1.403(7) . ?
C53 H53 0.9300 . ?
C53 C54 1.386(7) . ?
C54 C55 1.469(7) . ?
C55 C56 1.370(6) . ?
C55 C64 1.421(7) . ?
C56 H56 0.9300 . ?
C56 C57 1.415(7) . ?
C57 H57 0.9300 . ?
C57 C58 1.365(8) . ?
C58 H58 0.9300 . ?
C58 C59 1.422(7) . ?
C59 C60 1.418(7) . ?
C59 C64 1.397(7) . ?
C60 H60 0.9300 . ?
C60 C61 1.363(8) . ?
C61 H61 0.9300 . ?
C61 C62 1.414(8) . ?
C62 H62 0.9300 . ?
C62 C63 1.372(7) . ?
C63 C64 1.409(6) . ?
C65 C66 1.377(6) . ?
C65 C70 1.406(6) . ?
C65 C79 1.487(6) . ?
C66 H66 0.9300 . ?
C66 C67 1.387(7) . ?
C67 H67 0.9300 . ?
C67 C68 1.375(7) . ?
C68 H68 0.9300 . ?
C68 C69 1.386(7) . ?
C69 H69 0.9300 . ?
C69 C70 1.387(6) . ?
C70 C71 1.480(6) . ?
C71 C72 1.378(6) . ?
C71 C80 1.411(6) . ?
C72 H72 0.9300 . ?
C72 C73 1.420(7) . ?
C73 H73 0.9300 . ?
C73 C74 1.366(7) . ?
C74 H74 0.9300 . ?
C74 C75 1.415(7) . ?
C75 C76 1.416(7) . ?
C75 C80 1.397(6) . ?
C76 H76 0.9300 . ?
C76 C77 1.375(7) . ?
C77 H77 0.9300 . ?
C77 C78 1.425(6) . ?
C78 H78 0.9300 . ?
C78 C79 1.374(6) . ?
C79 C80 1.407(6) . ?
C81 C82 1.384(6) . ?
C81 C86 1.424(6) . ?
C81 C95 1.470(6) . ?
C82 H82 0.9300 . ?
C82 C83 1.382(7) . ?
C83 H83 0.9300 . ?
C83 C84 1.375(7) . ?
C84 H84 0.9300 . ?
C84 C85 1.390(7) . ?
C85 H85 0.9300 . ?
C85 C86 1.381(7) . ?
C86 C87 1.467(7) . ?
C87 C88 1.375(7) . ?
C87 C96 1.411(8) . ?
C88 H88 0.9300 . ?
C88 C89 1.399(10) . ?
C89 H89 0.9300 . ?
C89 C90 1.330(11) . ?
C90 H90 0.9300 . ?
C90 C91 1.455(10) . ?
C91 C92 1.396(10) . ?
C91 C96 1.415(8) . ?
C92 H92 0.9300 . ?
C92 C93 1.367(10) . ?
C93 H93 0.9300 . ?
C93 C94 1.434(8) . ?
C94 H94 0.9300 . ?
C94 C95 1.371(7) . ?
C95 C96 1.416(7) . ?
C97 C98 1.394(7) . ?
C97 C102 1.418(7) . ?
C97 C111 1.468(7) . ?
C98 H98 0.9300 . ?
C98 C99 1.387(9) . ?
C99 H99 0.9300 . ?
C99 C100 1.381(9) . ?
C100 H100 0.9300 . ?
C100 C101 1.385(8) . ?
C101 H101 0.9300 . ?
C101 C102 1.393(8) . ?
C102 C103 1.454(7) . ?
C103 C104 1.403(7) . ?
C103 C112 1.394(7) . ?
C104 H104 0.9300 . ?
C104 C105 1.403(8) . ?
C105 H105 0.9300 . ?
C105 C106 1.372(8) . ?
C106 H106 0.9300 . ?
C106 C107 1.416(7) . ?
C107 C108 1.419(7) . ?
C107 C112 1.394(7) . ?
C108 H108 0.9300 . ?
C108 C109 1.379(7) . ?
C109 H109 0.9300 . ?
C109 C110 1.413(8) . ?
C110 H110 0.9300 . ?
C110 C111 1.371(7) . ?
C111 C112 1.420(7) . ?
C113 C114 1.389(6) . ?
C113 C118 1.417(7) . ?
C113 C127 1.480(7) . ?
C114 H114 0.9300 . ?
C114 C115 1.382(7) . ?
C115 H115 0.9300 . ?
C115 C116 1.392(7) . ?
C116 H116 0.9300 . ?
C116 C117 1.392(7) . ?
C117 H117 0.9300 . ?
C117 C118 1.393(7) . ?
C118 C119 1.469(6) . ?
C119 C120 1.369(6) . ?
C119 C128 1.416(7) . ?
C120 H120 0.9300 . ?
C120 C121 1.425(7) . ?
C121 H121 0.9300 . ?
C121 C122 1.367(7) . ?
C122 H122 0.9300 . ?
C122 C123 1.432(7) . ?
C123 C124 1.415(7) . ?
C123 C128 1.394(6) . ?
C124 H124 0.9300 . ?
C124 C125 1.363(7) . ?
C125 H125 0.9300 . ?
C125 C126 1.429(7) . ?
C126 H126 0.9300 . ?
C126 C127 1.360(7) . ?
C127 C128 1.416(6) . ?
C129 C130 1.402(8) . ?
C129 C134 1.443(8) . ?
C129 C143 1.444(9) . ?
C130 H130 0.9300 . ?
C130 C131 1.363(11) . ?
C131 H131 0.9300 . ?
C131 C132 1.388(10) . ?
C132 H132 0.9300 . ?
C132 C133 1.409(8) . ?
C133 H133 0.9300 . ?
C133 C134 1.363(8) . ?
C134 C135 1.484(7) . ?
C135 C136 1.372(6) . ?
C135 C144 1.408(8) . ?
C136 H136 0.9300 . ?
C136 C137 1.402(7) . ?
C137 H137 0.9300 . ?
C137 C138 1.381(7) . ?
C138 H138 0.9300 . ?
C138 C139 1.421(7) . ?
C139 C140 1.427(8) . ?
C139 C144 1.397(8) . ?
C140 H140 0.9300 . ?
C140 C141 1.376(8) . ?
C141 H141 0.9300 . ?
C141 C142 1.394(9) . ?
C142 H142 0.9300 . ?
C142 C143 1.388(9) . ?
C143 C144 1.413(7) . ?
C145 C146 1.380(6) . ?
C145 C150 1.418(6) . ?
C145 C159 1.474(6) . ?
C146 H146 0.9300 . ?
C146 C147 1.387(7) . ?
C147 H147 0.9300 . ?
C147 C148 1.388(7) . ?
C148 H148 0.9300 . ?
C148 C149 1.395(7) . ?
C149 H149 0.9300 . ?
C149 C150 1.374(6) . ?
C150 C151 1.487(6) . ?
C151 C152 1.366(6) . ?
C151 C160 1.413(6) . ?
C152 H152 0.9300 . ?
C152 C153 1.420(6) . ?
C153 H153 0.9300 . ?
C153 C154 1.365(7) . ?
C154 H154 0.9300 . ?
C154 C155 1.428(7) . ?
C155 C156 1.429(7) . ?
C155 C160 1.398(6) . ?
C156 H156 0.9300 . ?
C156 C157 1.359(7) . ?
C157 H157 0.9300 . ?
C157 C158 1.417(7) . ?
C158 H158 0.9300 . ?
C158 C159 1.372(6) . ?
C159 C160 1.415(6) . ?
C161 C162 1.393(6) . ?
C161 C166 1.415(7) . ?
C161 C175 1.479(7) . ?
C162 H162 0.9300 . ?
C162 C163 1.399(7) . ?
C163 H163 0.9300 . ?
C163 C164 1.384(7) . ?
C164 H164 0.9300 . ?
C164 C165 1.393(7) . ?
C165 H165 0.9300 . ?
C165 C166 1.387(7) . ?
C166 C167 1.481(6) . ?
C167 C168 1.385(6) . ?
C167 C176 1.418(7) . ?
C168 H168 0.9300 . ?
C168 C169 1.408(7) . ?
C169 H169 0.9300 . ?
C169 C170 1.368(7) . ?
C170 H170 0.9300 . ?
C170 C171 1.421(7) . ?
C171 C172 1.419(7) . ?
C171 C176 1.400(6) . ?
C172 H172 0.9300 . ?
C172 C173 1.382(7) . ?
C173 H173 0.9300 . ?
C173 C174 1.411(7) . ?
C174 H174 0.9300 . ?
C174 C175 1.364(7) . ?
C175 C176 1.408(6) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 I1 123.6(3) . . ?
C6 C1 C2 118.5(4) . . ?
C6 C1 I1 117.9(3) . . ?
C1 C2 I2 122.7(3) . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 I2 118.2(3) . . ?
C4 C3 C2 122.0(4) . . ?
F1 C3 C2 120.3(4) . . ?
F1 C3 C4 117.7(4) . . ?
C3 C4 C5 119.2(4) . . ?
F2 C4 C3 121.0(4) . . ?
F2 C4 C5 119.7(4) . . ?
C4 C5 C6 119.6(4) . . ?
F3 C5 C4 120.3(4) . . ?
F3 C5 C6 120.1(4) . . ?
C1 C6 C5 121.7(4) . . ?
F4 C6 C1 120.9(4) . . ?
F4 C6 C5 117.4(4) . . ?
C8 C7 I3 122.9(3) . . ?
C12 C7 C8 118.6(4) . . ?
C12 C7 I3 118.5(3) . . ?
C7 C8 I4 123.2(4) . . ?
C9 C8 C7 119.0(5) . . ?
C9 C8 I4 117.7(4) . . ?
C10 C9 C8 121.9(5) . . ?
F5 C9 C8 120.4(5) . . ?
F5 C9 C10 117.7(4) . . ?
C9 C10 C11 119.4(4) . . ?
F6 C10 C9 120.3(5) . . ?
F6 C10 C11 120.2(5) . . ?
C10 C11 C12 119.9(5) . . ?
F7 C11 C10 119.4(5) . . ?
F7 C11 C12 120.7(5) . . ?
C11 C12 C7 121.2(5) . . ?
F8 C12 C7 120.8(4) . . ?
F8 C12 C11 118.0(5) . . ?
C14 C13 I5 123.2(3) . . ?
C18 C13 C14 118.8(4) . . ?
C18 C13 I5 118.0(4) . . ?
C13 C14 I6 123.6(3) . . ?
C15 C14 C13 118.8(4) . . ?
C15 C14 I6 117.6(4) . . ?
C16 C15 C14 121.6(5) . . ?
F9 C15 C14 121.0(4) . . ?
F9 C15 C16 117.5(4) . . ?
C17 C16 C15 119.5(4) . . ?
F10 C16 C15 120.2(5) . . ?
F10 C16 C17 120.3(5) . . ?
C16 C17 C18 119.6(5) . . ?
F11 C17 C16 119.7(4) . . ?
F11 C17 C18 120.8(5) . . ?
C17 C18 C13 121.8(5) . . ?
F12 C18 C13 121.3(4) . . ?
F12 C18 C17 116.9(4) . . ?
C20 C19 I7 123.0(3) . . ?
C24 C19 C20 119.1(4) . . ?
C24 C19 I7 117.8(4) . . ?
C19 C20 I8 123.6(3) . . ?
C21 C20 C19 119.0(4) . . ?
C21 C20 I8 117.3(4) . . ?
C20 C21 C22 121.7(5) . . ?
F13 C21 C20 121.3(4) . . ?
F13 C21 C22 117.0(4) . . ?
C23 C22 C21 119.6(4) . . ?
F14 C22 C21 120.6(4) . . ?
F14 C22 C23 119.9(4) . . ?
C22 C23 C24 119.6(4) . . ?
F15 C23 C22 120.3(4) . . ?
F15 C23 C24 120.1(4) . . ?
C19 C24 C23 121.0(5) . . ?
F16 C24 C19 121.1(4) . . ?
F16 C24 C23 117.9(4) . . ?
C26 C25 I9 124.2(4) . . ?
C30 C25 C26 118.5(4) . . ?
C30 C25 I9 117.3(3) . . ?
C25 C26 I10 122.3(4) . . ?
C27 C26 C25 119.0(5) . . ?
C27 C26 I10 118.7(4) . . ?
C28 C27 C26 121.2(5) . . ?
F17 C27 C26 120.1(6) . . ?
F17 C27 C28 118.7(5) . . ?
C29 C28 C27 119.8(5) . . ?
F18 C28 C27 120.5(6) . . ?
F18 C28 C29 119.6(6) . . ?
C28 C29 C30 120.2(5) . . ?
F19 C29 C28 120.0(5) . . ?
F19 C29 C30 119.8(5) . . ?
C29 C30 C25 121.2(5) . . ?
F20 C30 C25 120.9(4) . . ?
F20 C30 C29 117.9(5) . . ?
C32 C31 I11 124.9(4) . . ?
C36 C31 C32 118.9(4) . . ?
C36 C31 I11 116.1(3) . . ?
C31 C32 I12 122.7(3) . . ?
C33 C32 C31 119.3(5) . . ?
C33 C32 I12 118.0(4) . . ?
C34 C33 C32 121.4(4) . . ?
F21 C33 C32 120.9(5) . . ?
F21 C33 C34 117.7(4) . . ?
C33 C34 C35 120.0(4) . . ?
F22 C34 C33 120.9(4) . . ?
F22 C34 C35 119.0(4) . . ?
C36 C35 C34 118.6(5) . . ?
F23 C35 C34 120.1(4) . . ?
F23 C35 C36 121.3(5) . . ?
C35 C36 C31 121.7(5) . . ?
F24 C36 C31 122.0(4) . . ?
F24 C36 C35 116.3(5) . . ?
C38 C37 I13 123.7(3) . . ?
C42 C37 C38 118.1(4) . . ?
C42 C37 I13 118.2(3) . . ?
C37 C38 I14 122.5(3) . . ?
C39 C38 C37 119.2(4) . . ?
C39 C38 I14 118.3(3) . . ?
C38 C39 C40 121.4(4) . . ?
F28 C39 C38 120.8(4) . . ?
F28 C39 C40 117.9(4) . . ?
C41 C40 C39 119.1(4) . . ?
F27 C40 C39 119.8(4) . . ?
F27 C40 C41 121.0(4) . . ?
C42 C41 C40 120.2(4) . . ?
F26 C41 C40 119.5(4) . . ?
F26 C41 C42 120.3(4) . . ?
C41 C42 C37 122.0(4) . . ?
F25 C42 C37 120.5(4) . . ?
F25 C42 C41 117.5(4) . . ?
C44 C43 I15 122.8(3) . . ?
C48 C43 C44 119.3(4) . . ?
C48 C43 I15 117.9(3) . . ?
C43 C44 C45 118.0(4) . . ?
C43 C44 I16 124.6(3) . . ?
C45 C44 I16 117.5(3) . . ?
C46 C45 C44 122.5(4) . . ?
F29 C45 C44 119.7(4) . . ?
F29 C45 C46 117.8(4) . . ?
C45 C46 C47 118.9(4) . . ?
F30 C46 C45 120.7(4) . . ?
F30 C46 C47 120.4(4) . . ?
C46 C47 C48 119.8(4) . . ?
F31 C47 C46 119.5(4) . . ?
F31 C47 C48 120.7(4) . . ?
C43 C48 C47 121.5(4) . . ?
F32 C48 C43 121.0(4) . . ?
F32 C48 C47 117.5(4) . . ?
C50 C49 C54 120.0(5) . . ?
C50 C49 C63 131.9(5) . . ?
C54 C49 C63 108.1(4) . . ?
C49 C50 H50 120.5 . . ?
C51 C50 C49 119.0(5) . . ?
C51 C50 H50 120.5 . . ?
C50 C51 H51 119.3 . . ?
C52 C51 C50 121.4(5) . . ?
C52 C51 H51 119.3 . . ?
C51 C52 H52 119.5 . . ?
C51 C52 C53 121.0(6) . . ?
C53 C52 H52 119.5 . . ?
C52 C53 H53 120.7 . . ?
C54 C53 C52 118.7(5) . . ?
C54 C53 H53 120.7 . . ?
C49 C54 C55 108.1(4) . . ?
C53 C54 C49 119.9(5) . . ?
C53 C54 C55 132.0(5) . . ?
C56 C55 C54 136.2(5) . . ?
C56 C55 C64 117.7(5) . . ?
C64 C55 C54 106.1(4) . . ?
C55 C56 H56 120.5 . . ?
C55 C56 C57 119.0(5) . . ?
C57 C56 H56 120.5 . . ?
C56 C57 H57 118.7 . . ?
C58 C57 C56 122.7(5) . . ?
C58 C57 H57 118.7 . . ?
C57 C58 H58 119.7 . . ?
C57 C58 C59 120.6(5) . . ?
C59 C58 H58 119.7 . . ?
C60 C59 C58 128.6(5) . . ?
C64 C59 C58 115.3(5) . . ?
C64 C59 C60 116.1(5) . . ?
C59 C60 H60 119.9 . . ?
C61 C60 C59 120.1(5) . . ?
C61 C60 H60 119.9 . . ?
C60 C61 H61 118.6 . . ?
C60 C61 C62 122.9(5) . . ?
C62 C61 H61 118.6 . . ?
C61 C62 H62 120.7 . . ?
C63 C62 C61 118.6(5) . . ?
C63 C62 H62 120.7 . . ?
C62 C63 C49 135.3(5) . . ?
C62 C63 C64 118.3(5) . . ?
C64 C63 C49 106.4(4) . . ?
C59 C64 C55 124.6(4) . . ?
C59 C64 C63 124.1(5) . . ?
C63 C64 C55 111.3(4) . . ?
C66 C65 C70 120.7(4) . . ?
C66 C65 C79 131.3(5) . . ?
C70 C65 C79 107.9(4) . . ?
C65 C66 H66 120.6 . . ?
C65 C66 C67 118.7(5) . . ?
C67 C66 H66 120.6 . . ?
C66 C67 H67 119.6 . . ?
C68 C67 C66 120.8(5) . . ?
C68 C67 H67 119.6 . . ?
C67 C68 H68 119.5 . . ?
C67 C68 C69 121.1(5) . . ?
C69 C68 H68 119.5 . . ?
C68 C69 H69 120.6 . . ?
C68 C69 C70 118.7(5) . . ?
C70 C69 H69 120.6 . . ?
C65 C70 C71 108.5(4) . . ?
C69 C70 C65 119.8(4) . . ?
C69 C70 C71 131.7(4) . . ?
C72 C71 C70 135.6(4) . . ?
C72 C71 C80 118.5(4) . . ?
C80 C71 C70 105.9(4) . . ?
C71 C72 H72 120.9 . . ?
C71 C72 C73 118.1(5) . . ?
C73 C72 H72 120.9 . . ?
C72 C73 H73 118.7 . . ?
C74 C73 C72 122.7(5) . . ?
C74 C73 H73 118.7 . . ?
C73 C74 H74 119.6 . . ?
C73 C74 C75 120.7(5) . . ?
C75 C74 H74 119.6 . . ?
C76 C75 C74 128.6(5) . . ?
C80 C75 C74 115.6(5) . . ?
C80 C75 C76 115.7(5) . . ?
C75 C76 H76 119.6 . . ?
C77 C76 C75 120.8(4) . . ?
C77 C76 H76 119.6 . . ?
C76 C77 H77 118.8 . . ?
C76 C77 C78 122.5(5) . . ?
C78 C77 H77 118.8 . . ?
C77 C78 H78 121.2 . . ?
C79 C78 C77 117.6(5) . . ?
C79 C78 H78 121.2 . . ?
C78 C79 C65 134.5(4) . . ?
C78 C79 C80 119.5(4) . . ?
C80 C79 C65 106.0(4) . . ?
C75 C80 C71 124.3(5) . . ?
C75 C80 C79 123.9(4) . . ?
C79 C80 C71 111.7(4) . . ?
C82 C81 C86 119.9(4) . . ?
C82 C81 C95 132.1(4) . . ?
C86 C81 C95 108.1(4) . . ?
C81 C82 H82 120.2 . . ?
C83 C82 C81 119.6(5) . . ?
C83 C82 H82 120.2 . . ?
C82 C83 H83 119.8 . . ?
C84 C83 C82 120.5(5) . . ?
C84 C83 H83 119.8 . . ?
C83 C84 H84 119.4 . . ?
C83 C84 C85 121.3(5) . . ?
C85 C84 H84 119.4 . . ?
C84 C85 H85 120.5 . . ?
C86 C85 C84 119.1(5) . . ?
C86 C85 H85 120.5 . . ?
C81 C86 C87 108.5(5) . . ?
C85 C86 C81 119.7(4) . . ?
C85 C86 C87 131.8(5) . . ?
C88 C87 C86 135.2(6) . . ?
C88 C87 C96 119.1(6) . . ?
C96 C87 C86 105.7(4) . . ?
C87 C88 H88 120.9 . . ?
C87 C88 C89 118.2(7) . . ?
C89 C88 H88 120.9 . . ?
C88 C89 H89 118.3 . . ?
C90 C89 C88 123.4(7) . . ?
C90 C89 H89 118.3 . . ?
C89 C90 H90 119.0 . . ?
C89 C90 C91 122.0(7) . . ?
C91 C90 H90 119.0 . . ?
C92 C91 C90 131.7(7) . . ?
C92 C91 C96 115.1(6) . . ?
C96 C91 C90 113.2(7) . . ?
C91 C92 H92 118.8 . . ?
C93 C92 C91 122.4(6) . . ?
C93 C92 H92 118.8 . . ?
C92 C93 H93 119.2 . . ?
C92 C93 C94 121.6(6) . . ?
C94 C93 H93 119.2 . . ?
C93 C94 H94 121.0 . . ?
C95 C94 C93 118.1(6) . . ?
C95 C94 H94 121.0 . . ?
C94 C95 C81 135.4(5) . . ?
C94 C95 C96 119.0(5) . . ?
C96 C95 C81 105.6(4) . . ?
C87 C96 C91 124.1(6) . . ?
C87 C96 C95 112.1(4) . . ?
C91 C96 C95 123.8(6) . . ?
C98 C97 C102 120.7(6) . . ?
C98 C97 C111 132.0(6) . . ?
C102 C97 C111 107.3(4) . . ?
C97 C98 H98 120.7 . . ?
C99 C98 C97 118.5(6) . . ?
C99 C98 H98 120.7 . . ?
C98 C99 H99 119.7 . . ?
C100 C99 C98 120.5(6) . . ?
C100 C99 H99 119.7 . . ?
C99 C100 H100 118.9 . . ?
C99 C100 C101 122.2(6) . . ?
C101 C100 H100 118.9 . . ?
C100 C101 H101 120.9 . . ?
C100 C101 C102 118.3(6) . . ?
C102 C101 H101 120.9 . . ?
C97 C102 C103 108.4(5) . . ?
C101 C102 C97 119.8(5) . . ?
C101 C102 C103 131.8(5) . . ?
C104 C103 C102 135.4(5) . . ?
C112 C103 C102 107.3(4) . . ?
C112 C103 C104 117.3(5) . . ?
C103 C104 H104 121.2 . . ?
C103 C104 C105 117.6(5) . . ?
C105 C104 H104 121.2 . . ?
C104 C105 H105 118.1 . . ?
C106 C105 C104 123.7(5) . . ?
C106 C105 H105 118.1 . . ?
C105 C106 H106 119.8 . . ?
C105 C106 C107 120.3(6) . . ?
C107 C106 H106 119.8 . . ?
C106 C107 C108 128.3(6) . . ?
C112 C107 C106 114.7(5) . . ?
C112 C107 C108 117.0(5) . . ?
C107 C108 H108 120.1 . . ?
C109 C108 C107 119.7(5) . . ?
C109 C108 H108 120.1 . . ?
C108 C109 H109 118.7 . . ?
C108 C109 C110 122.6(5) . . ?
C110 C109 H109 118.7 . . ?
C109 C110 H110 120.7 . . ?
C111 C110 C109 118.7(5) . . ?
C111 C110 H110 120.7 . . ?
C110 C111 C97 134.6(5) . . ?
C110 C111 C112 118.9(5) . . ?
C112 C111 C97 106.5(5) . . ?
C103 C112 C107 126.3(5) . . ?
C103 C112 C111 110.6(5) . . ?
C107 C112 C111 123.1(5) . . ?
C114 C113 C118 120.2(5) . . ?
C114 C113 C127 131.7(5) . . ?
C118 C113 C127 108.1(4) . . ?
C113 C114 H114 120.3 . . ?
C115 C114 C113 119.3(5) . . ?
C115 C114 H114 120.3 . . ?
C114 C115 H115 119.6 . . ?
C114 C115 C116 120.9(5) . . ?
C116 C115 H115 119.6 . . ?
C115 C116 H116 119.7 . . ?
C117 C116 C115 120.6(5) . . ?
C117 C116 H116 119.7 . . ?
C116 C117 H117 120.4 . . ?
C116 C117 C118 119.1(5) . . ?
C118 C117 H117 120.4 . . ?
C113 C118 C119 108.3(4) . . ?
C117 C118 C113 119.9(4) . . ?
C117 C118 C119 131.9(5) . . ?
C120 C119 C118 135.4(5) . . ?
C120 C119 C128 118.1(4) . . ?
C128 C119 C118 106.4(4) . . ?
C119 C120 H120 120.6 . . ?
C119 C120 C121 118.8(5) . . ?
C121 C120 H120 120.6 . . ?
C120 C121 H121 118.8 . . ?
C122 C121 C120 122.3(5) . . ?
C122 C121 H121 118.8 . . ?
C121 C122 H122 119.6 . . ?
C121 C122 C123 120.8(5) . . ?
C123 C122 H122 119.6 . . ?
C124 C123 C122 128.7(5) . . ?
C128 C123 C122 115.1(5) . . ?
C128 C123 C124 116.3(4) . . ?
C123 C124 H124 119.8 . . ?
C125 C124 C123 120.4(5) . . ?
C125 C124 H124 119.8 . . ?
C124 C125 H125 118.9 . . ?
C124 C125 C126 122.2(5) . . ?
C126 C125 H125 118.9 . . ?
C125 C126 H126 120.6 . . ?
C127 C126 C125 118.8(5) . . ?
C127 C126 H126 120.6 . . ?
C126 C127 C113 135.5(4) . . ?
C126 C127 C128 118.4(4) . . ?
C128 C127 C113 106.1(4) . . ?
C119 C128 C127 111.2(4) . . ?
C123 C128 C119 125.0(4) . . ?
C123 C128 C127 123.9(4) . . ?
C130 C129 C134 117.7(7) . . ?
C130 C129 C143 133.0(7) . . ?
C134 C129 C143 109.3(5) . . ?
C129 C130 H130 120.1 . . ?
C131 C130 C129 119.8(7) . . ?
C131 C130 H130 120.1 . . ?
C130 C131 H131 118.9 . . ?
C130 C131 C132 122.2(7) . . ?
C132 C131 H131 118.9 . . ?
C131 C132 H132 120.1 . . ?
C131 C132 C133 119.9(8) . . ?
C133 C132 H132 120.1 . . ?
C132 C133 H133 120.7 . . ?
C134 C133 C132 118.6(7) . . ?
C134 C133 H133 120.7 . . ?
C129 C134 C135 105.7(5) . . ?
C133 C134 C129 121.9(6) . . ?
C133 C134 C135 132.4(6) . . ?
C136 C135 C134 134.8(5) . . ?
C136 C135 C144 117.8(5) . . ?
C144 C135 C134 107.4(4) . . ?
C135 C136 H136 120.2 . . ?
C135 C136 C137 119.6(5) . . ?
C137 C136 H136 120.2 . . ?
C136 C137 H137 118.9 . . ?
C138 C137 C136 122.3(5) . . ?
C138 C137 H137 118.9 . . ?
C137 C138 H138 120.0 . . ?
C137 C138 C139 119.9(5) . . ?
C139 C138 H138 120.0 . . ?
C138 C139 C140 128.1(6) . . ?
C144 C139 C138 116.0(5) . . ?
C144 C139 C140 116.0(5) . . ?
C139 C140 H140 120.4 . . ?
C141 C140 C139 119.2(7) . . ?
C141 C140 H140 120.4 . . ?
C140 C141 H141 118.1 . . ?
C140 C141 C142 123.8(6) . . ?
C142 C141 H141 118.1 . . ?
C141 C142 H142 120.6 . . ?
C143 C142 C141 118.9(5) . . ?
C143 C142 H142 120.6 . . ?
C142 C143 C129 135.8(6) . . ?
C142 C143 C144 117.4(6) . . ?
C144 C143 C129 106.8(5) . . ?
C135 C144 C143 110.8(6) . . ?
C139 C144 C135 124.4(5) . . ?
C139 C144 C143 124.8(6) . . ?
C146 C145 C150 120.7(4) . . ?
C146 C145 C159 131.1(4) . . ?
C150 C145 C159 108.2(4) . . ?
C145 C146 H146 121.0 . . ?
C145 C146 C147 118.0(5) . . ?
C147 C146 H146 121.0 . . ?
C146 C147 H147 119.1 . . ?
C146 C147 C148 121.9(5) . . ?
C148 C147 H147 119.1 . . ?
C147 C148 H148 119.9 . . ?
C147 C148 C149 120.2(4) . . ?
C149 C148 H148 119.9 . . ?
C148 C149 H149 120.6 . . ?
C150 C149 C148 118.8(4) . . ?
C150 C149 H149 120.6 . . ?
C145 C150 C151 108.2(4) . . ?
C149 C150 C145 120.6(4) . . ?
C149 C150 C151 131.2(4) . . ?
C152 C151 C150 135.1(4) . . ?
C152 C151 C160 119.3(4) . . ?
C160 C151 C150 105.5(4) . . ?
C151 C152 H152 120.8 . . ?
C151 C152 C153 118.3(4) . . ?
C153 C152 H152 120.8 . . ?
C152 C153 H153 118.8 . . ?
C154 C153 C152 122.4(4) . . ?
C154 C153 H153 118.8 . . ?
C153 C154 H154 119.6 . . ?
C153 C154 C155 120.7(5) . . ?
C155 C154 H154 119.6 . . ?
C156 C155 C154 128.6(5) . . ?
C160 C155 C154 115.6(4) . . ?
C160 C155 C156 115.8(4) . . ?
C155 C156 H156 120.2 . . ?
C157 C156 C155 119.6(4) . . ?
C157 C156 H156 120.2 . . ?
C156 C157 H157 118.1 . . ?
C156 C157 C158 123.8(4) . . ?
C158 C157 H157 118.1 . . ?
C157 C158 H158 120.9 . . ?
C159 C158 C157 118.2(4) . . ?
C159 C158 H158 120.9 . . ?
C158 C159 C145 135.8(4) . . ?
C158 C159 C160 118.2(4) . . ?
C160 C159 C145 106.0(4) . . ?
C151 C160 C159 112.0(4) . . ?
C155 C160 C151 123.6(4) . . ?
C155 C160 C159 124.4(4) . . ?
C162 C161 C166 119.8(5) . . ?
C162 C161 C175 130.9(5) . . ?
C166 C161 C175 109.2(4) . . ?
C161 C162 H162 120.7 . . ?
C161 C162 C163 118.5(5) . . ?
C163 C162 H162 120.7 . . ?
C162 C163 H163 119.2 . . ?
C164 C163 C162 121.6(5) . . ?
C164 C163 H163 119.2 . . ?
C163 C164 H164 119.9 . . ?
C163 C164 C165 120.1(5) . . ?
C165 C164 H164 119.9 . . ?
C164 C165 H165 120.4 . . ?
C166 C165 C164 119.3(5) . . ?
C166 C165 H165 120.4 . . ?
C161 C166 C167 107.5(4) . . ?
C165 C166 C161 120.7(4) . . ?
C165 C166 C167 131.9(5) . . ?
C168 C167 C166 135.5(5) . . ?
C168 C167 C176 118.6(5) . . ?
C176 C167 C166 105.9(4) . . ?
C167 C168 H168 121.0 . . ?
C167 C168 C169 118.0(5) . . ?
C169 C168 H168 121.0 . . ?
C168 C169 H169 118.2 . . ?
C170 C169 C168 123.7(5) . . ?
C170 C169 H169 118.2 . . ?
C169 C170 H170 120.1 . . ?
C169 C170 C171 119.7(5) . . ?
C171 C170 H170 120.1 . . ?
C172 C171 C170 128.0(5) . . ?
C176 C171 C170 116.5(5) . . ?
C176 C171 C172 115.5(4) . . ?
C171 C172 H172 120.0 . . ?
C173 C172 C171 120.0(5) . . ?
C173 C172 H172 120.0 . . ?
C172 C173 H173 118.5 . . ?
C172 C173 C174 123.0(5) . . ?
C174 C173 H173 118.5 . . ?
C173 C174 H174 121.0 . . ?
C175 C174 C173 118.1(4) . . ?
C175 C174 H174 121.0 . . ?
C174 C175 C161 135.6(4) . . ?
C174 C175 C176 119.2(5) . . ?
C176 C175 C161 105.2(4) . . ?
C171 C176 C167 123.5(4) . . ?
C171 C176 C175 124.3(5) . . ?
C175 C176 C167 112.2(4) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -1.3(6) . . . . ?
C1 C2 C3 F1 -179.7(4) . . . . ?
C2 C1 C6 C5 -0.4(6) . . . . ?
C2 C1 C6 F4 179.1(4) . . . . ?
C2 C3 C4 C5 1.1(7) . . . . ?
C2 C3 C4 F2 -176.5(4) . . . . ?
C3 C4 C5 C6 -0.5(6) . . . . ?
C3 C4 C5 F3 179.3(4) . . . . ?
C4 C5 C6 C1 0.2(7) . . . . ?
C4 C5 C6 F4 -179.3(4) . . . . ?
C6 C1 C2 C3 0.9(6) . . . . ?
C6 C1 C2 I2 -179.3(3) . . . . ?
C7 C8 C9 C10 -1.2(7) . . . . ?
C7 C8 C9 F5 178.9(4) . . . . ?
C8 C7 C12 C11 1.1(7) . . . . ?
C8 C7 C12 F8 -179.7(4) . . . . ?
C8 C9 C10 C11 0.6(7) . . . . ?
C8 C9 C10 F6 -178.0(4) . . . . ?
C9 C10 C11 C12 0.8(7) . . . . ?
C9 C10 C11 F7 179.8(4) . . . . ?
C10 C11 C12 C7 -1.7(7) . . . . ?
C10 C11 C12 F8 179.1(4) . . . . ?
C12 C7 C8 C9 0.3(6) . . . . ?
C12 C7 C8 I4 178.8(3) . . . . ?
C13 C14 C15 C16 -2.0(6) . . . . ?
C13 C14 C15 F9 178.1(3) . . . . ?
C14 C13 C18 C17 0.7(6) . . . . ?
C14 C13 C18 F12 -179.0(3) . . . . ?
C14 C15 C16 C17 2.9(6) . . . . ?
C14 C15 C16 F10 -179.2(4) . . . . ?
C15 C16 C17 C18 -2.0(6) . . . . ?
C15 C16 C17 F11 177.4(3) . . . . ?
C16 C17 C18 C13 0.2(6) . . . . ?
C16 C17 C18 F12 179.9(4) . . . . ?
C18 C13 C14 C15 0.2(6) . . . . ?
C18 C13 C14 I6 179.6(3) . . . . ?
C19 C20 C21 C22 0.1(6) . . . . ?
C19 C20 C21 F13 179.1(3) . . . . ?
C20 C19 C24 C23 2.1(6) . . . . ?
C20 C19 C24 F16 -179.7(3) . . . . ?
C20 C21 C22 C23 1.6(6) . . . . ?
C20 C21 C22 F14 -178.7(4) . . . . ?
C21 C22 C23 C24 -1.4(6) . . . . ?
C21 C22 C23 F15 177.4(4) . . . . ?
C22 C23 C24 C19 -0.4(6) . . . . ?
C22 C23 C24 F16 -178.7(3) . . . . ?
C24 C19 C20 C21 -1.9(6) . . . . ?
C24 C19 C20 I8 -178.8(3) . . . . ?
C25 C26 C27 C28 0.8(6) . . . . ?
C25 C26 C27 F17 -179.6(4) . . . . ?
C26 C25 C30 C29 0.4(6) . . . . ?
C26 C25 C30 F20 179.5(3) . . . . ?
C26 C27 C28 C29 -0.2(7) . . . . ?
C26 C27 C28 F18 179.8(4) . . . . ?
C27 C28 C29 C30 -0.2(7) . . . . ?
C27 C28 C29 F19 178.5(4) . . . . ?
C28 C29 C30 C25 0.1(6) . . . . ?
C28 C29 C30 F20 -179.0(4) . . . . ?
C30 C25 C26 C27 -0.8(6) . . . . ?
C30 C25 C26 I10 178.0(3) . . . . ?
C31 C32 C33 C34 0.1(6) . . . . ?
C31 C32 C33 F21 -179.7(3) . . . . ?
C32 C31 C36 C35 -0.8(6) . . . . ?
C32 C31 C36 F24 177.9(3) . . . . ?
C32 C33 C34 C35 0.4(6) . . . . ?
C32 C33 C34 F22 -179.6(4) . . . . ?
C33 C34 C35 C36 -1.1(6) . . . . ?
C33 C34 C35 F23 179.0(4) . . . . ?
C34 C35 C36 C31 1.3(6) . . . . ?
C34 C35 C36 F24 -177.5(3) . . . . ?
C36 C31 C32 C33 0.1(6) . . . . ?
C36 C31 C32 I12 -177.2(3) . . . . ?
C37 C38 C39 C40 0.1(7) . . . . ?
C37 C38 C39 F28 -179.5(4) . . . . ?
C38 C37 C42 C41 -0.2(7) . . . . ?
C38 C37 C42 F25 -179.8(4) . . . . ?
C38 C39 C40 C41 0.6(7) . . . . ?
C38 C39 C40 F27 -177.7(4) . . . . ?
C39 C40 C41 C42 -1.1(7) . . . . ?
C39 C40 C41 F26 178.6(4) . . . . ?
C40 C41 C42 C37 1.0(7) . . . . ?
C40 C41 C42 F25 -179.5(4) . . . . ?
C42 C37 C38 C39 -0.3(6) . . . . ?
C42 C37 C38 I14 -178.9(3) . . . . ?
C43 C44 C45 C46 -2.7(7) . . . . ?
C43 C44 C45 F29 178.5(4) . . . . ?
C44 C43 C48 C47 -0.1(7) . . . . ?
C44 C43 C48 F32 -179.5(4) . . . . ?
C44 C45 C46 C47 3.4(7) . . . . ?
C44 C45 C46 F30 -177.7(4) . . . . ?
C45 C46 C47 C48 -2.4(7) . . . . ?
C45 C46 C47 F31 176.8(4) . . . . ?
C46 C47 C48 C43 0.8(7) . . . . ?
C46 C47 C48 F32 -179.8(4) . . . . ?
C48 C43 C44 C45 1.0(6) . . . . ?
C48 C43 C44 I16 179.5(3) . . . . ?
C49 C50 C51 C52 -0.3(7) . . . . ?
C49 C54 C55 C56 178.3(5) . . . . ?
C49 C54 C55 C64 -0.7(5) . . . . ?
C49 C63 C64 C55 1.0(5) . . . . ?
C49 C63 C64 C59 -179.0(4) . . . . ?
C50 C49 C54 C53 1.6(6) . . . . ?
C50 C49 C54 C55 -179.0(4) . . . . ?
C50 C49 C63 C62 -0.7(9) . . . . ?
C50 C49 C63 C64 178.9(5) . . . . ?
C50 C51 C52 C53 -0.3(8) . . . . ?
C51 C52 C53 C54 1.5(7) . . . . ?
C52 C53 C54 C49 -2.1(6) . . . . ?
C52 C53 C54 C55 178.7(4) . . . . ?
C53 C54 C55 C56 -2.5(9) . . . . ?
C53 C54 C55 C64 178.6(5) . . . . ?
C54 C49 C50 C51 -0.4(7) . . . . ?
C54 C49 C63 C62 178.9(5) . . . . ?
C54 C49 C63 C64 -1.5(5) . . . . ?
C54 C55 C56 C57 -179.8(5) . . . . ?
C54 C55 C64 C59 179.8(4) . . . . ?
C54 C55 C64 C63 -0.2(5) . . . . ?
C55 C56 C57 C58 1.0(7) . . . . ?
C56 C55 C64 C59 0.6(7) . . . . ?
C56 C55 C64 C63 -179.4(4) . . . . ?
C56 C57 C58 C59 -0.6(7) . . . . ?
C57 C58 C59 C60 -178.7(5) . . . . ?
C57 C58 C59 C64 0.2(6) . . . . ?
C58 C59 C60 C61 179.3(5) . . . . ?
C58 C59 C64 C55 -0.2(6) . . . . ?
C58 C59 C64 C63 179.8(4) . . . . ?
C59 C60 C61 C62 0.7(7) . . . . ?
C60 C59 C64 C55 178.8(4) . . . . ?
C60 C59 C64 C63 -1.2(6) . . . . ?
C60 C61 C62 C63 -1.1(7) . . . . ?
C61 C62 C63 C49 -180.0(5) . . . . ?
C61 C62 C63 C64 0.4(7) . . . . ?
C62 C63 C64 C55 -179.2(4) . . . . ?
C62 C63 C64 C59 0.7(7) . . . . ?
C63 C49 C50 C51 179.2(5) . . . . ?
C63 C49 C54 C53 -178.0(4) . . . . ?
C63 C49 C54 C55 1.3(5) . . . . ?
C64 C55 C56 C57 -0.9(6) . . . . ?
C64 C59 C60 C61 0.5(7) . . . . ?
C65 C66 C67 C68 -0.7(6) . . . . ?
C65 C70 C71 C72 177.3(4) . . . . ?
C65 C70 C71 C80 -0.5(4) . . . . ?
C65 C79 C80 C71 1.3(4) . . . . ?
C65 C79 C80 C75 -179.5(4) . . . . ?
C66 C65 C70 C69 3.1(6) . . . . ?
C66 C65 C70 C71 -178.2(4) . . . . ?
C66 C65 C79 C78 -1.6(8) . . . . ?
C66 C65 C79 C80 177.9(4) . . . . ?
C66 C67 C68 C69 1.2(7) . . . . ?
C67 C68 C69 C70 0.5(6) . . . . ?
C68 C69 C70 C65 -2.6(6) . . . . ?
C68 C69 C70 C71 179.1(4) . . . . ?
C69 C70 C71 C72 -4.3(8) . . . . ?
C69 C70 C71 C80 177.9(4) . . . . ?
C70 C65 C66 C67 -1.4(6) . . . . ?
C70 C65 C79 C78 179.0(4) . . . . ?
C70 C65 C79 C80 -1.5(4) . . . . ?
C70 C71 C72 C73 -179.4(4) . . . . ?
C70 C71 C80 C75 -179.8(4) . . . . ?
C70 C71 C80 C79 -0.5(4) . . . . ?
C71 C72 C73 C74 0.4(7) . . . . ?
C72 C71 C80 C75 2.0(6) . . . . ?
C72 C71 C80 C79 -178.8(4) . . . . ?
C72 C73 C74 C75 1.2(7) . . . . ?
C73 C74 C75 C76 177.7(4) . . . . ?
C73 C74 C75 C80 -1.1(6) . . . . ?
C74 C75 C76 C77 179.5(4) . . . . ?
C74 C75 C80 C71 -0.5(6) . . . . ?
C74 C75 C80 C79 -179.6(4) . . . . ?
C75 C76 C77 C78 0.7(7) . . . . ?
C76 C75 C80 C71 -179.4(4) . . . . ?
C76 C75 C80 C79 1.4(6) . . . . ?
C76 C77 C78 C79 0.9(6) . . . . ?
C77 C78 C79 C65 178.1(4) . . . . ?
C77 C78 C79 C80 -1.3(6) . . . . ?
C78 C79 C80 C71 -179.2(4) . . . . ?
C78 C79 C80 C75 0.1(6) . . . . ?
C79 C65 C66 C67 179.2(4) . . . . ?
C79 C65 C70 C69 -177.4(3) . . . . ?
C79 C65 C70 C71 1.2(4) . . . . ?
C80 C71 C72 C73 -1.8(6) . . . . ?
C80 C75 C76 C77 -1.8(6) . . . . ?
C81 C82 C83 C84 -0.4(7) . . . . ?
C81 C86 C87 C88 176.8(5) . . . . ?
C81 C86 C87 C96 -0.7(5) . . . . ?
C81 C95 C96 C87 0.1(5) . . . . ?
C81 C95 C96 C91 -179.3(4) . . . . ?
C82 C81 C86 C85 1.4(6) . . . . ?
C82 C81 C86 C87 -179.1(4) . . . . ?
C82 C81 C95 C94 -0.5(9) . . . . ?
C82 C81 C95 C96 179.2(5) . . . . ?
C82 C83 C84 C85 1.2(7) . . . . ?
C83 C84 C85 C86 -0.6(7) . . . . ?
C84 C85 C86 C81 -0.6(7) . . . . ?
C84 C85 C86 C87 179.9(5) . . . . ?
C85 C86 C87 C88 -3.7(9) . . . . ?
C85 C86 C87 C96 178.8(5) . . . . ?
C86 C81 C82 C83 -0.9(6) . . . . ?
C86 C81 C95 C94 179.7(5) . . . . ?
C86 C81 C95 C96 -0.5(5) . . . . ?
C86 C87 C88 C89 -178.4(5) . . . . ?
C86 C87 C96 C91 179.7(4) . . . . ?
C86 C87 C96 C95 0.3(5) . . . . ?
C87 C88 C89 C90 0.6(10) . . . . ?
C88 C87 C96 C91 1.8(8) . . . . ?
C88 C87 C96 C95 -177.6(4) . . . . ?
C88 C89 C90 C91 -0.6(11) . . . . ?
C89 C90 C91 C92 178.6(7) . . . . ?
C89 C90 C91 C96 1.0(9) . . . . ?
C90 C91 C92 C93 -177.7(6) . . . . ?
C90 C91 C96 C87 -1.6(7) . . . . ?
C90 C91 C96 C95 177.7(5) . . . . ?
C91 C92 C93 C94 0.5(9) . . . . ?
C92 C91 C96 C87 -179.6(5) . . . . ?
C92 C91 C96 C95 -0.3(8) . . . . ?
C92 C93 C94 C95 -0.3(8) . . . . ?
C93 C94 C95 C81 179.5(5) . . . . ?
C93 C94 C95 C96 -0.2(7) . . . . ?
C94 C95 C96 C87 179.9(4) . . . . ?
C94 C95 C96 C91 0.5(7) . . . . ?
C95 C81 C82 C83 179.4(4) . . . . ?
C95 C81 C86 C85 -178.8(4) . . . . ?
C95 C81 C86 C87 0.7(5) . . . . ?
C96 C87 C88 C89 -1.2(8) . . . . ?
C96 C91 C92 C93 -0.2(8) . . . . ?
C97 C98 C99 C100 -0.1(8) . . . . ?
C97 C102 C103 C104 178.2(5) . . . . ?
C97 C102 C103 C112 0.7(5) . . . . ?
C97 C111 C112 C103 0.3(5) . . . . ?
C97 C111 C112 C107 -179.4(4) . . . . ?
C98 C97 C102 C101 0.6(6) . . . . ?
C98 C97 C102 C103 -179.1(4) . . . . ?
C98 C97 C111 C110 0.4(8) . . . . ?
C98 C97 C111 C112 178.5(5) . . . . ?
C98 C99 C100 C101 0.2(8) . . . . ?
C99 C100 C101 C102 0.1(8) . . . . ?
C100 C101 C102 C97 -0.5(7) . . . . ?
C100 C101 C102 C103 179.2(5) . . . . ?
C101 C102 C103 C104 -1.5(9) . . . . ?
C101 C102 C103 C112 -179.0(4) . . . . ?
C102 C97 C98 C99 -0.4(7) . . . . ?
C102 C97 C111 C110 -177.9(5) . . . . ?
C102 C97 C111 C112 0.1(4) . . . . ?
C102 C103 C104 C105 -178.2(5) . . . . ?
C102 C103 C112 C107 179.1(4) . . . . ?
C102 C103 C112 C111 -0.6(5) . . . . ?
C103 C104 C105 C106 1.0(7) . . . . ?
C104 C103 C112 C107 1.1(6) . . . . ?
C104 C103 C112 C111 -178.7(4) . . . . ?
C104 C105 C106 C107 -1.2(7) . . . . ?
C105 C106 C107 C108 179.2(4) . . . . ?
C105 C106 C107 C112 1.2(6) . . . . ?
C106 C107 C108 C109 -177.2(4) . . . . ?
C106 C107 C112 C103 -1.2(6) . . . . ?
C106 C107 C112 C111 178.5(4) . . . . ?
C107 C108 C109 C110 -1.1(7) . . . . ?
C108 C107 C112 C103 -179.4(4) . . . . ?
C108 C107 C112 C111 0.3(6) . . . . ?
C108 C109 C110 C111 0.4(7) . . . . ?
C109 C110 C111 C97 178.5(4) . . . . ?
C109 C110 C111 C112 0.7(6) . . . . ?
C110 C111 C112 C103 178.7(4) . . . . ?
C110 C111 C112 C107 -1.0(6) . . . . ?
C111 C97 C98 C99 -178.5(4) . . . . ?
C111 C97 C102 C101 179.2(4) . . . . ?
C111 C97 C102 C103 -0.5(5) . . . . ?
C112 C103 C104 C105 -0.9(6) . . . . ?
C112 C107 C108 C109 0.8(6) . . . . ?
C113 C114 C115 C116 1.5(7) . . . . ?
C113 C118 C119 C120 -178.4(5) . . . . ?
C113 C118 C119 C128 -0.9(5) . . . . ?
C113 C127 C128 C119 -1.1(5) . . . . ?
C113 C127 C128 C123 179.9(4) . . . . ?
C114 C113 C118 C117 -1.0(6) . . . . ?
C114 C113 C118 C119 -179.8(4) . . . . ?
C114 C113 C127 C126 1.3(9) . . . . ?
C114 C113 C127 C128 -179.4(5) . . . . ?
C114 C115 C116 C117 -2.1(7) . . . . ?
C115 C116 C117 C118 1.1(7) . . . . ?
C116 C117 C118 C113 0.4(7) . . . . ?
C116 C117 C118 C119 178.9(4) . . . . ?
C117 C118 C119 C120 3.0(9) . . . . ?
C117 C118 C119 C128 -179.5(5) . . . . ?
C118 C113 C114 C115 0.0(7) . . . . ?
C118 C113 C127 C126 -178.8(5) . . . . ?
C118 C113 C127 C128 0.5(5) . . . . ?
C118 C119 C120 C121 179.1(5) . . . . ?
C118 C119 C128 C123 -179.8(4) . . . . ?
C118 C119 C128 C127 1.3(5) . . . . ?
C119 C120 C121 C122 -1.2(7) . . . . ?
C120 C119 C128 C123 -1.8(7) . . . . ?
C120 C119 C128 C127 179.3(4) . . . . ?
C120 C121 C122 C123 0.4(8) . . . . ?
C121 C122 C123 C124 179.8(5) . . . . ?
C121 C122 C123 C128 -0.3(7) . . . . ?
C122 C123 C124 C125 -179.9(5) . . . . ?
C122 C123 C128 C119 1.0(7) . . . . ?
C122 C123 C128 C127 179.7(4) . . . . ?
C123 C124 C125 C126 0.9(7) . . . . ?
C124 C123 C128 C119 -179.1(4) . . . . ?
C124 C123 C128 C127 -0.3(7) . . . . ?
C124 C125 C126 C127 -1.8(7) . . . . ?
C125 C126 C127 C113 -179.1(5) . . . . ?
C125 C126 C127 C128 1.6(7) . . . . ?
C126 C127 C128 C119 178.3(4) . . . . ?
C126 C127 C128 C123 -0.6(7) . . . . ?
C127 C113 C114 C115 180.0(4) . . . . ?
C127 C113 C118 C117 179.0(4) . . . . ?
C127 C113 C118 C119 0.2(5) . . . . ?
C128 C119 C120 C121 1.8(7) . . . . ?
C128 C123 C124 C125 0.2(7) . . . . ?
C129 C130 C131 C132 0.1(8) . . . . ?
C129 C134 C135 C136 -179.4(4) . . . . ?
C129 C134 C135 C144 -0.4(4) . . . . ?
C129 C143 C144 C135 0.0(5) . . . . ?
C129 C143 C144 C139 179.3(4) . . . . ?
C130 C129 C134 C133 0.0(6) . . . . ?
C130 C129 C134 C135 -179.4(4) . . . . ?
C130 C129 C143 C142 -2.3(9) . . . . ?
C130 C129 C143 C144 179.5(5) . . . . ?
C130 C131 C132 C133 -0.1(8) . . . . ?
C131 C132 C133 C134 0.0(7) . . . . ?
C132 C133 C134 C129 0.0(7) . . . . ?
C132 C133 C134 C135 179.2(4) . . . . ?
C133 C134 C135 C136 1.3(8) . . . . ?
C133 C134 C135 C144 -179.7(5) . . . . ?
C134 C129 C130 C131 -0.1(7) . . . . ?
C134 C129 C143 C142 178.0(5) . . . . ?
C134 C129 C143 C144 -0.2(5) . . . . ?
C134 C135 C136 C137 -179.9(4) . . . . ?
C134 C135 C144 C139 -179.1(4) . . . . ?
C134 C135 C144 C143 0.2(5) . . . . ?
C135 C136 C137 C138 -1.0(6) . . . . ?
C136 C135 C144 C139 0.1(6) . . . . ?
C136 C135 C144 C143 179.5(4) . . . . ?
C136 C137 C138 C139 -0.4(6) . . . . ?
C137 C138 C139 C140 -179.0(4) . . . . ?
C137 C138 C139 C144 1.6(6) . . . . ?
C138 C139 C140 C141 -179.5(4) . . . . ?
C138 C139 C144 C135 -1.5(6) . . . . ?
C138 C139 C144 C143 179.3(4) . . . . ?
C139 C140 C141 C142 -0.1(7) . . . . ?
C140 C139 C144 C135 179.0(4) . . . . ?
C140 C139 C144 C143 -0.2(6) . . . . ?
C140 C141 C142 C143 0.5(7) . . . . ?
C141 C142 C143 C129 -178.9(5) . . . . ?
C141 C142 C143 C144 -0.8(7) . . . . ?
C142 C143 C144 C135 -178.7(4) . . . . ?
C142 C143 C144 C139 0.7(6) . . . . ?
C143 C129 C130 C131 -179.8(5) . . . . ?
C143 C129 C134 C133 179.8(4) . . . . ?
C143 C129 C134 C135 0.4(5) . . . . ?
C144 C135 C136 C137 1.1(6) . . . . ?
C144 C139 C140 C141 -0.1(6) . . . . ?
C145 C146 C147 C148 0.0(7) . . . . ?
C145 C150 C151 C152 177.7(5) . . . . ?
C145 C150 C151 C160 0.6(5) . . . . ?
C145 C159 C160 C151 0.0(5) . . . . ?
C145 C159 C160 C155 -179.1(4) . . . . ?
C146 C145 C150 C149 -0.5(7) . . . . ?
C146 C145 C150 C151 179.1(4) . . . . ?
C146 C145 C159 C158 3.1(9) . . . . ?
C146 C145 C159 C160 -179.2(5) . . . . ?
C146 C147 C148 C149 -0.8(7) . . . . ?
C147 C148 C149 C150 0.9(7) . . . . ?
C148 C149 C150 C145 -0.2(7) . . . . ?
C148 C149 C150 C151 -179.7(4) . . . . ?
C149 C150 C151 C152 -2.7(9) . . . . ?
C149 C150 C151 C160 -179.9(5) . . . . ?
C150 C145 C146 C147 0.6(7) . . . . ?
C150 C145 C159 C158 -177.4(5) . . . . ?
C150 C145 C159 C160 0.4(5) . . . . ?
C150 C151 C152 C153 -178.0(4) . . . . ?
C150 C151 C160 C155 178.7(4) . . . . ?
C150 C151 C160 C159 -0.3(5) . . . . ?
C151 C152 C153 C154 0.3(7) . . . . ?
C152 C151 C160 C155 1.1(6) . . . . ?
C152 C151 C160 C159 -178.0(4) . . . . ?
C152 C153 C154 C155 0.8(7) . . . . ?
C153 C154 C155 C156 177.0(5) . . . . ?
C153 C154 C155 C160 -0.9(6) . . . . ?
C154 C155 C156 C157 -178.3(5) . . . . ?
C154 C155 C160 C151 0.0(6) . . . . ?
C154 C155 C160 C159 179.0(4) . . . . ?
C155 C156 C157 C158 0.2(7) . . . . ?
C156 C155 C160 C151 -178.2(4) . . . . ?
C156 C155 C160 C159 0.8(6) . . . . ?
C156 C157 C158 C159 -0.3(7) . . . . ?
C157 C158 C159 C145 178.1(5) . . . . ?
C157 C158 C159 C160 0.6(6) . . . . ?
C158 C159 C160 C151 178.2(4) . . . . ?
C158 C159 C160 C155 -0.9(7) . . . . ?
C159 C145 C146 C147 -179.8(4) . . . . ?
C159 C145 C150 C149 179.8(4) . . . . ?
C159 C145 C150 C151 -0.6(5) . . . . ?
C160 C151 C152 C153 -1.2(6) . . . . ?
C160 C155 C156 C157 -0.4(6) . . . . ?
C161 C162 C163 C164 0.6(6) . . . . ?
C161 C166 C167 C168 -177.8(4) . . . . ?
C161 C166 C167 C176 0.7(4) . . . . ?
C161 C175 C176 C167 0.5(4) . . . . ?
C161 C175 C176 C171 179.2(4) . . . . ?
C162 C161 C166 C165 -1.0(6) . . . . ?
C162 C161 C166 C167 179.4(4) . . . . ?
C162 C161 C175 C174 -1.3(8) . . . . ?
C162 C161 C175 C176 -179.8(4) . . . . ?
C162 C163 C164 C165 -0.7(7) . . . . ?
C163 C164 C165 C166 -0.1(6) . . . . ?
C164 C165 C166 C161 0.9(6) . . . . ?
C164 C165 C166 C167 -179.6(4) . . . . ?
C165 C166 C167 C168 2.7(8) . . . . ?
C165 C166 C167 C176 -178.8(4) . . . . ?
C166 C161 C162 C163 0.2(6) . . . . ?
C166 C161 C175 C174 178.5(5) . . . . ?
C166 C161 C175 C176 0.0(4) . . . . ?
C166 C167 C168 C169 178.5(4) . . . . ?
C166 C167 C176 C171 -179.5(4) . . . . ?
C166 C167 C176 C175 -0.7(5) . . . . ?
C167 C168 C169 C170 0.5(6) . . . . ?
C168 C167 C176 C171 -0.7(6) . . . . ?
C168 C167 C176 C175 178.0(4) . . . . ?
C168 C169 C170 C171 -0.7(7) . . . . ?
C169 C170 C171 C172 -177.3(4) . . . . ?
C169 C170 C171 C176 0.2(6) . . . . ?
C170 C171 C172 C173 177.3(4) . . . . ?
C170 C171 C176 C167 0.5(6) . . . . ?
C170 C171 C176 C175 -178.1(4) . . . . ?
C171 C172 C173 C174 0.6(6) . . . . ?
C172 C171 C176 C167 178.3(4) . . . . ?
C172 C171 C176 C175 -0.3(6) . . . . ?
C172 C173 C174 C175 -0.5(6) . . . . ?
C173 C174 C175 C161 -178.3(4) . . . . ?
C173 C174 C175 C176 0.0(6) . . . . ?
C174 C175 C176 C167 -178.3(4) . . . . ?
C174 C175 C176 C171 0.4(6) . . . . ?
C175 C161 C162 C163 -180.0(4) . . . . ?
C175 C161 C166 C165 179.1(4) . . . . ?
C175 C161 C166 C167 -0.4(4) . . . . ?
C176 C167 C168 C169 0.2(6) . . . . ?
C176 C171 C172 C173 -0.2(6) . . . . ?
F1 C3 C4 C5 179.5(4) . . . . ?
F1 C3 C4 F2 2.0(6) . . . . ?
F2 C4 C5 C6 177.1(4) . . . . ?
F2 C4 C5 F3 -3.1(6) . . . . ?
F3 C5 C6 C1 -179.6(4) . . . . ?
F3 C5 C6 F4 0.9(6) . . . . ?
F5 C9 C10 C11 -179.5(4) . . . . ?
F5 C9 C10 F6 1.8(6) . . . . ?
F6 C10 C11 C12 179.5(4) . . . . ?
F6 C10 C11 F7 -1.5(7) . . . . ?
F7 C11 C12 C7 179.3(4) . . . . ?
F7 C11 C12 F8 0.1(6) . . . . ?
F9 C15 C16 C17 -177.1(4) . . . . ?
F9 C15 C16 F10 0.7(6) . . . . ?
F10 C16 C17 C18 -179.8(4) . . . . ?
F10 C16 C17 F11 -0.5(6) . . . . ?
F11 C17 C18 C13 -179.1(4) . . . . ?
F11 C17 C18 F12 0.6(6) . . . . ?
F13 C21 C22 C23 -177.4(3) . . . . ?
F13 C21 C22 F14 2.3(6) . . . . ?
F14 C22 C23 C24 178.9(3) . . . . ?
F14 C22 C23 F15 -2.3(6) . . . . ?
F15 C23 C24 C19 -179.2(3) . . . . ?
F15 C23 C24 F16 2.5(6) . . . . ?
F17 C27 C28 C29 -179.8(4) . . . . ?
F17 C27 C28 F18 0.2(6) . . . . ?
F18 C28 C29 C30 179.7(4) . . . . ?
F18 C28 C29 F19 -1.6(6) . . . . ?
F19 C29 C30 C25 -178.6(4) . . . . ?
F19 C29 C30 F20 2.4(6) . . . . ?
F21 C33 C34 C35 -179.8(4) . . . . ?
F21 C33 C34 F22 0.2(6) . . . . ?
F22 C34 C35 C36 178.9(4) . . . . ?
F22 C34 C35 F23 -1.1(6) . . . . ?
F23 C35 C36 C31 -178.7(4) . . . . ?
F23 C35 C36 F24 2.4(6) . . . . ?
F26 C41 C42 C37 -178.8(4) . . . . ?
F26 C41 C42 F25 0.8(6) . . . . ?
F27 C40 C41 C42 177.1(4) . . . . ?
F27 C40 C41 F26 -3.2(6) . . . . ?
F28 C39 C40 C41 -179.7(4) . . . . ?
F28 C39 C40 F27 2.0(6) . . . . ?
F29 C45 C46 C47 -177.7(4) . . . . ?
F29 C45 C46 F30 1.2(6) . . . . ?
F30 C46 C47 C48 178.7(4) . . . . ?
F30 C46 C47 F31 -2.2(6) . . . . ?
F31 C47 C48 C43 -178.3(4) . . . . ?
F31 C47 C48 F32 1.1(6) . . . . ?
I1 C1 C2 C3 179.8(3) . . . . ?
I1 C1 C2 I2 -0.4(5) . . . . ?
I1 C1 C6 C5 -179.3(3) . . . . ?
I1 C1 C6 F4 0.1(5) . . . . ?
I2 C2 C3 C4 178.9(3) . . . . ?
I2 C2 C3 F1 0.5(5) . . . . ?
I3 C7 C8 C9 179.9(3) . . . . ?
I3 C7 C8 I4 -1.6(5) . . . . ?
I3 C7 C12 C11 -178.4(3) . . . . ?
I3 C7 C12 F8 0.7(6) . . . . ?
I4 C8 C9 C10 -179.8(3) . . . . ?
I4 C8 C9 F5 0.3(6) . . . . ?
I5 C13 C14 C15 -178.6(3) . . . . ?
I5 C13 C14 I6 0.7(5) . . . . ?
I5 C13 C18 C17 179.5(3) . . . . ?
I5 C13 C18 F12 -0.2(5) . . . . ?
I6 C14 C15 C16 178.6(3) . . . . ?
I6 C14 C15 F9 -1.3(5) . . . . ?
I7 C19 C20 C21 179.8(3) . . . . ?
I7 C19 C20 I8 2.9(5) . . . . ?
I7 C19 C24 C23 -179.5(3) . . . . ?
I7 C19 C24 F16 -1.2(5) . . . . ?
I8 C20 C21 C22 177.2(3) . . . . ?
I8 C20 C21 F13 -3.8(5) . . . . ?
I9 C25 C26 C27 -179.5(3) . . . . ?
I9 C25 C26 I10 -0.6(5) . . . . ?
I9 C25 C30 C29 179.2(3) . . . . ?
I9 C25 C30 F20 -1.8(5) . . . . ?
I10 C26 C27 C28 -178.2(3) . . . . ?
I10 C26 C27 F17 1.4(5) . . . . ?
I11 C31 C32 C33 -179.7(3) . . . . ?
I11 C31 C32 I12 2.9(5) . . . . ?
I11 C31 C36 C35 179.0(3) . . . . ?
I11 C31 C36 F24 -2.2(5) . . . . ?
I12 C32 C33 C34 177.6(3) . . . . ?
I12 C32 C33 F21 -2.2(5) . . . . ?
I13 C37 C38 C39 -179.4(3) . . . . ?
I13 C37 C38 I14 2.0(5) . . . . ?
I13 C37 C42 C41 178.9(3) . . . . ?
I13 C37 C42 F25 -0.7(6) . . . . ?
I14 C38 C39 C40 178.8(3) . . . . ?
I14 C38 C39 F28 -0.9(6) . . . . ?
I15 C43 C44 C45 -178.1(3) . . . . ?
I15 C43 C44 I16 0.5(5) . . . . ?
I15 C43 C48 C47 179.1(3) . . . . ?
I15 C43 C48 F32 -0.3(6) . . . . ?
I16 C44 C45 C46 178.6(3) . . . . ?
I16 C44 C45 F29 -0.2(5) . . . . ?
_shelx_res_file
;
20161228b.res created by SHELXL-2014/7
TITL 20161228b_a.res in P-1
REM Old TITL 20161228b in P-1 #2
REM SHELXT solution in P-1
REM R1 0.159, Rweak 0.010, Alpha 0.063, Orientation as input
REM Formula found by SHELXT: C86 F30 I16
CELL 0.71073 15.296341 18.100933 30.480008 99.2518 90.4052 114.4204
ZERR 16 0.000327 0.000403 0.000498 0.0016 0.0015 0.0021
LATT 1
SFAC C H F I
UNIT 352 160 64 32
ISOR 0.01 0.02 $C
L.S. 15
PLAN 3
BOND $H
CONF
MORE -1
fmap 2
acta 52
OMIT 0 -1 22
OMIT 0 -1 24
OMIT 0 -1 26
REM
REM
REM
WGHT 0.014400 7.113200
FVAR 0.06995
C1 1 0.709946 1.038180 0.387162 11.00000 0.02287 0.01987 =
0.01246 0.00406 -0.00530 0.00699
C2 1 0.787553 1.024549 0.369269 11.00000 0.01322 0.01949 =
0.01760 0.00951 -0.00220 -0.00118
C3 1 0.770488 0.948055 0.344986 11.00000 0.02365 0.02460 =
0.01350 0.00799 0.00210 0.01129
C4 1 0.680546 0.884513 0.338481 11.00000 0.03210 0.01665 =
0.01247 0.00094 -0.00356 0.00861
C5 1 0.604057 0.897470 0.356103 11.00000 0.01960 0.02427 =
0.02169 0.00878 -0.00664 0.00098
C6 1 0.619790 0.974044 0.380242 11.00000 0.01889 0.02770 =
0.01736 0.00988 -0.00162 0.00964
C7 1 0.263062 0.066188 0.385710 11.00000 0.02161 0.02303 =
0.01071 0.00361 -0.00140 0.00978
C8 1 0.361642 0.107558 0.381225 11.00000 0.01802 0.02786 =
0.02037 0.01190 -0.00475 0.00408
C9 1 0.408653 0.064810 0.357867 11.00000 0.01865 0.04113 =
0.02128 0.01392 0.00183 0.01495
C10 1 0.361822 -0.017170 0.339723 11.00000 0.03911 0.03624 =
0.01746 0.00609 -0.00006 0.02507
C11 1 0.265271 -0.058357 0.344330 11.00000 0.04033 0.02537 =
0.01639 0.00692 -0.00495 0.00870
C12 1 0.216097 -0.016608 0.366667 11.00000 0.02031 0.03052 =
0.01832 0.01123 -0.00385 -0.00066
C13 1 0.253452 0.432818 0.125516 11.00000 0.02656 0.02099 =
0.01513 0.00488 0.00829 0.01001
C14 1 0.162157 0.406983 0.103787 11.00000 0.02135 0.01862 =
0.01387 0.00105 0.00548 0.00119
C15 1 0.122374 0.463249 0.104872 11.00000 0.01974 0.02473 =
0.01627 0.00256 0.00578 0.00623
C16 1 0.169330 0.543106 0.127968 11.00000 0.02955 0.02443 =
0.02328 0.00488 0.01143 0.01562
C17 1 0.259088 0.568494 0.148652 11.00000 0.03484 0.02454 =
0.01426 0.00291 0.01143 0.01112
C18 1 0.300254 0.513369 0.147343 11.00000 0.01934 0.02598 =
0.01333 0.00274 0.00174 0.00364
C19 1 0.252191 0.460763 0.376829 11.00000 0.02990 0.02074 =
0.00751 0.00327 0.00571 0.00861
C20 1 0.157907 0.440196 0.360728 11.00000 0.02028 0.02096 =
0.01507 0.00220 0.00318 0.00016
C21 1 0.130548 0.502181 0.356841 11.00000 0.01547 0.03474 =
0.01147 0.00210 0.00419 0.00496
C22 1 0.193676 0.583939 0.368348 11.00000 0.02587 0.02518 =
0.01285 -0.00065 0.00273 0.01181
C23 1 0.286744 0.604404 0.383053 11.00000 0.02864 0.01988 =
0.01389 0.00151 0.00675 0.00704
C24 1 0.315878 0.542644 0.387124 11.00000 0.01377 0.02746 =
0.01091 0.00107 0.00065 0.00155
C25 1 0.810858 0.445015 0.133409 11.00000 0.02865 0.01750 =
0.01449 0.00635 0.01104 0.01026
C26 1 0.740618 0.472205 0.123823 11.00000 0.03283 0.03793 =
0.02099 0.01891 0.01121 0.01876
C27 1 0.757418 0.553483 0.139810 11.00000 0.05606 0.05672 =
0.03228 0.03002 0.02689 0.04491
C28 1 0.841675 0.607528 0.164255 11.00000 0.06793 0.02639 =
0.02722 0.01183 0.02675 0.02608
C29 1 0.910559 0.581319 0.173327 11.00000 0.04294 0.01868 =
0.01782 0.00160 0.00968 0.00470
C30 1 0.895661 0.501209 0.158210 11.00000 0.02411 0.02274 =
0.01542 0.00749 0.00804 0.00542
C31 1 0.787309 0.471315 0.387338 11.00000 0.02867 0.01772 =
0.01298 0.00412 0.00579 0.00820
C32 1 0.730337 0.510228 0.377207 11.00000 0.01713 0.02497 =
0.01451 0.00592 0.00394 0.00545
C33 1 0.769401 0.595094 0.383795 11.00000 0.03017 0.02436 =
0.01548 0.00206 0.00708 0.01762
C34 1 0.863265 0.641840 0.400071 11.00000 0.02643 0.01780 =
0.01777 0.00565 0.00777 0.00768
C35 1 0.921255 0.604001 0.410035 11.00000 0.02033 0.03161 =
0.01846 0.00491 0.00543 0.00548
C36 1 0.881936 0.518984 0.403905 11.00000 0.03728 0.03094 =
0.01294 0.00865 0.01149 0.02190
C37 1 0.701679 1.005341 0.129748 11.00000 0.02676 0.01740 =
0.01352 0.00430 -0.00243 0.00881
C38 1 0.777568 0.986638 0.112928 11.00000 0.02357 0.02126 =
0.01188 0.00490 0.00082 0.00456
C39 1 0.761323 0.905414 0.099419 11.00000 0.02520 0.02463 =
0.01593 0.00322 -0.00079 0.01011
C40 1 0.672308 0.841800 0.101868 11.00000 0.02858 0.01971 =
0.01836 0.00560 -0.00064 0.00784
C41 1 0.598621 0.860472 0.117793 11.00000 0.02261 0.03340 =
0.01557 0.01361 0.00147 0.00928
C42 1 0.613850 0.940742 0.131678 11.00000 0.02373 0.03632 =
0.01416 0.01157 0.00655 0.01655
C43 1 0.263983 1.043120 0.130211 11.00000 0.02638 0.02506 =
0.01123 0.00099 -0.00414 0.01216
C44 1 0.357924 1.067106 0.117967 11.00000 0.03116 0.02408 =
0.00972 0.00489 -0.00198 0.00961
C45 1 0.386878 1.005356 0.100512 11.00000 0.02724 0.02787 =
0.01335 0.00914 0.00413 0.01379
C46 1 0.328359 0.923871 0.096840 11.00000 0.03125 0.03169 =
0.01354 0.00570 0.00010 0.01930
C47 1 0.235240 0.900990 0.108638 11.00000 0.02660 0.02383 =
0.01080 0.00177 -0.00763 0.00605
C48 1 0.204284 0.960542 0.125372 11.00000 0.01979 0.03167 =
0.01724 0.00685 0.00237 0.00898
C49 1 0.687414 1.013482 0.518091 11.00000 0.02787 0.02953 =
0.02226 0.01706 0.00673 0.01255
C50 1 0.639994 1.053050 0.544243 11.00000 0.04402 0.04673 =
0.02774 0.02369 0.01301 0.02401
AFIX 43
H50 2 0.573481 1.027664 0.545142 11.00000 -1.20000
AFIX 0
C51 1 0.693302 1.130911 0.568965 11.00000 0.07155 0.04495 =
0.02851 0.01714 0.01377 0.03854
AFIX 43
H51 2 0.661836 1.157763 0.586421 11.00000 -1.20000
AFIX 0
C52 1 0.791001 1.169076 0.568264 11.00000 0.07387 0.02552 =
0.02690 0.01080 -0.00070 0.01886
AFIX 43
H52 2 0.824847 1.221470 0.585115 11.00000 -1.20000
AFIX 0
C53 1 0.841143 1.130485 0.542516 11.00000 0.04265 0.02337 =
0.02619 0.01462 -0.00209 0.00326
AFIX 43
H53 2 0.907875 1.156228 0.542696 11.00000 -1.20000
AFIX 0
C54 1 0.789251 1.053204 0.516793 11.00000 0.03209 0.02324 =
0.02096 0.01436 0.00159 0.00801
C55 1 0.819078 0.998116 0.486139 11.00000 0.02148 0.02829 =
0.02111 0.01490 -0.00162 0.00791
C56 1 0.903916 1.001225 0.470334 11.00000 0.01820 0.04009 =
0.03293 0.01764 -0.00122 0.00871
AFIX 43
H56 2 0.961392 1.047508 0.479477 11.00000 -1.20000
AFIX 0
C57 1 0.902770 0.932945 0.439886 11.00000 0.03259 0.05876 =
0.03411 0.02238 0.00640 0.03189
AFIX 43
H57 2 0.960684 0.935006 0.429595 11.00000 -1.20000
AFIX 0
C58 1 0.820123 0.864197 0.425011 11.00000 0.05081 0.03487 =
0.02884 0.01077 0.00031 0.03037
AFIX 43
H58 2 0.822746 0.820985 0.404779 11.00000 -1.20000
AFIX 0
C59 1 0.730015 0.857977 0.440143 11.00000 0.03892 0.02850 =
0.02612 0.01413 -0.00234 0.01764
C60 1 0.637790 0.791444 0.429193 11.00000 0.05432 0.02191 =
0.02862 0.01078 -0.01380 0.00707
AFIX 43
H60 2 0.630998 0.744210 0.409423 11.00000 -1.20000
AFIX 0
C61 1 0.559094 0.796589 0.447587 11.00000 0.03661 0.03062 =
0.03362 0.01759 -0.01274 -0.00163
AFIX 43
H61 2 0.499477 0.751947 0.440137 11.00000 -1.20000
AFIX 0
C62 1 0.564132 0.866843 0.477506 11.00000 0.02198 0.03965 =
0.04421 0.02602 -0.00057 0.00548
AFIX 43
H62 2 0.508842 0.868733 0.489069 11.00000 -1.20000
AFIX 0
C63 1 0.652338 0.932178 0.489118 11.00000 0.02104 0.02888 =
0.02876 0.01939 -0.00045 0.00708
C64 1 0.733605 0.926167 0.470356 11.00000 0.02098 0.02477 =
0.02247 0.01527 -0.00238 0.00723
C65 1 0.811759 0.471941 0.513300 11.00000 0.02310 0.02140 =
0.00839 0.00488 0.00297 0.00788
C66 1 0.850056 0.417736 0.520476 11.00000 0.02231 0.03162 =
0.01084 0.00372 0.00130 0.01243
AFIX 43
H66 2 0.915608 0.436476 0.528128 11.00000 -1.20000
AFIX 0
C67 1 0.788986 0.334637 0.516073 11.00000 0.04405 0.03171 =
0.01688 0.00483 0.00438 0.02189
AFIX 43
H67 2 0.814048 0.297292 0.520495 11.00000 -1.20000
AFIX 0
C68 1 0.691866 0.306813 0.505252 11.00000 0.03409 0.01737 =
0.02018 0.00166 0.00778 0.00550
AFIX 43
H68 2 0.651977 0.251011 0.503022 11.00000 -1.20000
AFIX 0
C69 1 0.652434 0.360596 0.497612 11.00000 0.01914 0.03001 =
0.01390 0.00049 0.00233 0.00429
AFIX 43
H69 2 0.586608 0.341428 0.490517 11.00000 -1.20000
AFIX 0
C70 1 0.713020 0.443528 0.500752 11.00000 0.01720 0.02230 =
0.00837 0.00099 0.00398 0.00391
C71 1 0.693840 0.514880 0.494124 11.00000 0.01449 0.02759 =
0.00925 0.00227 0.00403 0.00768
C72 1 0.614596 0.525943 0.480656 11.00000 0.02168 0.03555 =
0.01788 0.00385 0.00598 0.01331
AFIX 43
H72 2 0.554840 0.481411 0.473372 11.00000 -1.20000
AFIX 0
C73 1 0.626746 0.607274 0.478211 11.00000 0.03590 0.04875 =
0.01775 0.00508 0.00342 0.02746
AFIX 43
H73 2 0.573532 0.615321 0.469315 11.00000 -1.20000
AFIX 0
C74 1 0.713430 0.674187 0.488396 11.00000 0.03957 0.03160 =
0.02234 0.00869 0.00829 0.02229
AFIX 43
H74 2 0.717679 0.726442 0.486829 11.00000 -1.20000
AFIX 0
C75 1 0.796838 0.664855 0.501306 11.00000 0.03055 0.02491 =
0.01464 0.00469 0.00913 0.01161
C76 1 0.892459 0.726015 0.511535 11.00000 0.04132 0.02061 =
0.02143 0.00292 0.01422 0.00818
AFIX 43
H76 2 0.906220 0.780512 0.509840 11.00000 -1.20000
AFIX 0
C77 1 0.965190 0.705770 0.523944 11.00000 0.02549 0.02305 =
0.02003 -0.00072 0.00727 -0.00375
AFIX 43
H77 2 1.027117 0.747397 0.530757 11.00000 -1.20000
AFIX 0
C78 1 0.949225 0.623386 0.526757 11.00000 0.02148 0.02117 =
0.01624 -0.00087 0.00378 0.00451
AFIX 43
H78 2 0.999167 0.611002 0.535617 11.00000 -1.20000
AFIX 0
C79 1 0.857332 0.562925 0.515898 11.00000 0.01832 0.01977 =
0.00918 0.00201 0.00552 0.00428
C80 1 0.783277 0.584353 0.503492 11.00000 0.01953 0.02276 =
0.01089 0.00602 0.00697 0.00782
C81 1 0.680323 1.007195 0.257448 11.00000 0.02151 0.02181 =
0.01057 0.00541 0.00029 0.00910
C82 1 0.635269 1.054910 0.277220 11.00000 0.02299 0.03061 =
0.01590 0.00338 -0.00069 0.01201
AFIX 43
H82 2 0.569757 1.030734 0.281059 11.00000 -1.20000
AFIX 0
C83 1 0.688217 1.138727 0.291233 11.00000 0.04444 0.03366 =
0.02499 0.00458 -0.00627 0.02265
AFIX 43
H83 2 0.658024 1.170985 0.304366 11.00000 -1.20000
AFIX 0
C84 1 0.785219 1.174738 0.285889 11.00000 0.04195 0.02454 =
0.02775 0.00867 -0.01261 0.00495
AFIX 43
H84 2 0.820017 1.231037 0.295992 11.00000 -1.20000
AFIX 0
C85 1 0.832279 1.128597 0.265672 11.00000 0.02346 0.04589 =
0.02704 0.02071 -0.00316 0.00293
AFIX 43
H85 2 0.897791 1.153765 0.261989 11.00000 -1.20000
AFIX 0
C86 1 0.780383 1.044860 0.251133 11.00000 0.02446 0.03254 =
0.01607 0.01103 0.00186 0.01326
C87 1 0.808793 0.980942 0.229008 11.00000 0.04233 0.06673 =
0.01496 0.01313 0.00289 0.03865
C88 1 0.892266 0.980090 0.213038 11.00000 0.04931 0.11952 =
0.02926 0.02084 0.00592 0.06052
AFIX 43
H88 2 0.948491 1.028424 0.215914 11.00000 -1.20000
AFIX 0
C89 1 0.890353 0.904544 0.192342 11.00000 0.09777 0.14963 =
0.03521 0.01717 0.00040 0.10169
AFIX 43
H89 2 0.946939 0.903796 0.181797 11.00000 -1.20000
AFIX 0
C90 1 0.811826 0.833761 0.186968 11.00000 0.13421 0.10469 =
0.03692 0.00492 -0.00250 0.10854
AFIX 43
H90 2 0.815402 0.785791 0.172664 11.00000 -1.20000
AFIX 0
C91 1 0.720476 0.829097 0.202791 11.00000 0.10469 0.06291 =
0.02697 0.00925 -0.00494 0.06496
C92 1 0.630012 0.763033 0.200094 11.00000 0.14181 0.04119 =
0.02680 0.00298 -0.01789 0.05318
AFIX 43
H92 2 0.623037 0.710661 0.186903 11.00000 -1.20000
AFIX 0
C93 1 0.551339 0.772503 0.216126 11.00000 0.10260 0.03034 =
0.02737 0.01407 -0.02000 0.00616
AFIX 43
H93 2 0.492714 0.726505 0.213739 11.00000 -1.20000
AFIX 0
C94 1 0.556992 0.851632 0.236535 11.00000 0.05589 0.02439 =
0.02328 0.00849 -0.01051 0.00323
AFIX 43
H94 2 0.502980 0.857478 0.247223 11.00000 -1.20000
AFIX 0
C95 1 0.644288 0.918394 0.239837 11.00000 0.03801 0.02575 =
0.01052 0.00772 -0.00263 0.01556
C96 1 0.724620 0.906527 0.223221 11.00000 0.05341 0.04368 =
0.01670 0.00675 -0.00176 0.03732
C97 1 0.815291 0.626656 0.275232 11.00000 0.03853 0.02778 =
0.01624 0.00387 0.01297 0.00534
C98 1 0.847373 0.711876 0.287184 11.00000 0.05484 0.04394 =
0.02633 0.00947 0.01295 0.01408
AFIX 43
H98 2 0.807753 0.737381 0.281577 11.00000 -1.20000
AFIX 0
C99 1 0.939668 0.757749 0.307617 11.00000 0.05557 0.03780 =
0.03420 0.00223 0.00933 -0.00745
AFIX 43
H99 2 0.962356 0.814677 0.315796 11.00000 -1.20000
AFIX 0
C100 1 0.998184 0.719542 0.315919 11.00000 0.03872 0.06474 =
0.02921 0.00445 0.00878 -0.00997
AFIX 43
H100 2 1.059726 0.751606 0.329761 11.00000 -1.20000
AFIX 0
C101 1 0.968210 0.635052 0.304305 11.00000 0.03029 0.05983 =
0.02454 0.00660 0.00642 0.01001
AFIX 43
H101 2 1.008676 0.610487 0.310205 11.00000 -1.20000
AFIX 0
C102 1 0.875904 0.587831 0.283561 11.00000 0.02145 0.05003 =
0.01447 0.00820 0.00730 0.00965
C103 1 0.824022 0.499759 0.267007 11.00000 0.02535 0.04161 =
0.01572 0.00828 0.00449 0.01692
C104 1 0.845235 0.430940 0.264561 11.00000 0.03162 0.05796 =
0.02172 0.01320 0.00629 0.02466
AFIX 43
H104 2 0.904468 0.436114 0.275938 11.00000 -1.20000
AFIX 0
C105 1 0.773877 0.354029 0.244335 11.00000 0.05439 0.03490 =
0.02589 0.01050 0.00802 0.02497
AFIX 43
H105 2 0.786968 0.307947 0.243010 11.00000 -1.20000
AFIX 0
C106 1 0.685888 0.342931 0.226401 11.00000 0.04826 0.03145 =
0.02443 0.00921 0.01192 0.01158
AFIX 43
H106 2 0.641887 0.290527 0.212894 11.00000 -1.20000
AFIX 0
C107 1 0.661703 0.410872 0.228348 11.00000 0.03544 0.04038 =
0.01676 0.00627 0.00847 0.01505
C108 1 0.575498 0.411579 0.211336 11.00000 0.02097 0.04100 =
0.02261 0.00188 0.00393 0.00816
AFIX 43
H108 2 0.524898 0.362581 0.197876 11.00000 -1.20000
AFIX 0
C109 1 0.567095 0.485232 0.214852 11.00000 0.02421 0.05940 =
0.02363 0.00839 0.00833 0.01910
AFIX 43
H109 2 0.510606 0.484810 0.203070 11.00000 -1.20000
AFIX 0
C110 1 0.640907 0.561333 0.235646 11.00000 0.04229 0.04770 =
0.02214 0.01250 0.01237 0.02820
AFIX 43
H110 2 0.632993 0.609989 0.237676 11.00000 -1.20000
AFIX 0
C111 1 0.724385 0.562010 0.252762 11.00000 0.02526 0.04206 =
0.01783 0.01320 0.01077 0.01778
C112 1 0.734007 0.486494 0.248561 11.00000 0.02446 0.02991 =
0.01385 0.00598 0.00903 0.01107
C113 1 0.321949 -0.027820 0.227496 11.00000 0.02480 0.02988 =
0.01194 0.00480 -0.00225 0.01077
C114 1 0.371182 -0.072606 0.208166 11.00000 0.03193 0.03717 =
0.01546 0.00654 0.00452 0.01842
AFIX 43
H114 2 0.436586 -0.046155 0.204536 11.00000 -1.20000
AFIX 0
C115 1 0.321985 -0.156888 0.194378 11.00000 0.05226 0.03515 =
0.01699 0.00361 0.00070 0.02761
AFIX 43
H115 2 0.355040 -0.187268 0.182078 11.00000 -1.20000
AFIX 0
C116 1 0.223598 -0.196906 0.198660 11.00000 0.04922 0.02601 =
0.02502 0.00708 -0.00434 0.01600
AFIX 43
H116 2 0.191231 -0.253365 0.188300 11.00000 -1.20000
AFIX 0
C117 1 0.173269 -0.153150 0.218308 11.00000 0.03064 0.03201 =
0.02095 0.01108 -0.00287 0.00795
AFIX 43
H117 2 0.107777 -0.180166 0.221599 11.00000 -1.20000
AFIX 0
C118 1 0.222269 -0.068339 0.232989 11.00000 0.03014 0.02787 =
0.01026 0.00675 -0.00168 0.01138
C119 1 0.189704 -0.006223 0.253934 11.00000 0.03163 0.03325 =
0.01254 0.00758 -0.00020 0.01682
C120 1 0.104388 -0.007554 0.268027 11.00000 0.02735 0.03930 =
0.02267 0.00671 0.00286 0.01451
AFIX 43
H120 2 0.049344 -0.056915 0.264622 11.00000 -1.20000
AFIX 0
C121 1 0.101462 0.068096 0.288014 11.00000 0.03180 0.06072 =
0.02421 0.00915 0.00394 0.03083
AFIX 43
H121 2 0.043255 0.067404 0.297096 11.00000 -1.20000
AFIX 0
C122 1 0.181203 0.141642 0.294304 11.00000 0.04883 0.03867 =
0.01882 0.00001 -0.00062 0.02862
AFIX 43
H122 2 0.176310 0.189591 0.307645 11.00000 -1.20000
AFIX 0
C123 1 0.272182 0.145695 0.280587 11.00000 0.03459 0.03514 =
0.01324 0.00431 -0.00256 0.01907
C124 1 0.361533 0.215572 0.284221 11.00000 0.04681 0.02523 =
0.01854 0.00278 -0.00225 0.01763
AFIX 43
H124 2 0.365838 0.267321 0.297007 11.00000 -1.20000
AFIX 0
C125 1 0.441306 0.207444 0.269086 11.00000 0.03525 0.03282 =
0.02443 0.00491 -0.00293 0.00671
AFIX 43
H125 2 0.499462 0.254070 0.272197 11.00000 -1.20000
AFIX 0
C126 1 0.438536 0.129642 0.248593 11.00000 0.02734 0.03031 =
0.02507 0.00759 0.00297 0.01156
AFIX 43
H126 2 0.493536 0.125920 0.237764 11.00000 -1.20000
AFIX 0
C127 1 0.354086 0.061161 0.245206 11.00000 0.02955 0.02832 =
0.01001 0.00647 0.00164 0.01325
C128 1 0.271798 0.070385 0.261140 11.00000 0.02606 0.02623 =
0.01214 0.00533 -0.00169 0.01268
C129 1 0.793357 0.598196 0.027831 11.00000 0.06931 0.02775 =
0.04432 0.02079 0.04431 0.02463
C130 1 0.817441 0.677357 0.052400 11.00000 0.10462 0.03125 =
0.05286 0.02373 0.05848 0.03244
AFIX 43
H130 2 0.776487 0.703156 0.050377 11.00000 -1.20000
AFIX 0
C131 1 0.901041 0.716413 0.079263 11.00000 0.11241 0.02773 =
0.04578 0.00994 0.05289 0.01227
AFIX 43
H131 2 0.916073 0.768876 0.095432 11.00000 -1.20000
AFIX 0
C132 1 0.964496 0.680471 0.083288 11.00000 0.07162 0.04683 =
0.04537 0.00927 0.03485 -0.00325
AFIX 43
H132 2 1.021025 0.708789 0.101885 11.00000 -1.20000
AFIX 0
C133 1 0.943094 0.601019 0.059146 11.00000 0.04867 0.03649 =
0.04005 0.00536 0.02508 0.00085
AFIX 43
H133 2 0.985012 0.576255 0.061542 11.00000 -1.20000
AFIX 0
C134 1 0.859656 0.561213 0.032204 11.00000 0.04781 0.02343 =
0.03154 0.01427 0.02960 0.01067
C135 1 0.816477 0.479421 0.002469 11.00000 0.03159 0.02295 =
0.02689 0.01261 0.01996 0.01354
C136 1 0.842408 0.415045 -0.008114 11.00000 0.02497 0.02798 =
0.02837 0.01172 0.01022 0.01333
AFIX 43
H136 2 0.899268 0.418047 0.004857 11.00000 -1.20000
AFIX 0
C137 1 0.782640 0.344700 -0.038610 11.00000 0.04099 0.02513 =
0.03060 0.01269 0.01457 0.02015
AFIX 43
H137 2 0.801424 0.301801 -0.045909 11.00000 -1.20000
AFIX 0
C138 1 0.696811 0.336917 -0.058188 11.00000 0.03494 0.02228 =
0.03329 0.01404 0.01295 0.01079
AFIX 43
H138 2 0.659069 0.289531 -0.078425 11.00000 -1.20000
AFIX 0
C139 1 0.666282 0.401395 -0.047364 11.00000 0.02818 0.03905 =
0.03300 0.02722 0.02121 0.01554
C140 1 0.580033 0.404169 -0.063472 11.00000 0.03563 0.05583 =
0.05146 0.03723 0.02300 0.02027
AFIX 43
H140 2 0.535333 0.359891 -0.083455 11.00000 -1.20000
AFIX 0
C141 1 0.563802 0.473124 -0.049086 11.00000 0.05332 0.07730 =
0.07337 0.05856 0.04003 0.04770
AFIX 43
H141 2 0.507296 0.473946 -0.059939 11.00000 -1.20000
AFIX 0
C142 1 0.627208 0.541833 -0.019171 11.00000 0.07250 0.05359 =
0.06363 0.04149 0.05301 0.04879
AFIX 43
H142 2 0.612742 0.586828 -0.010251 11.00000 -1.20000
AFIX 0
C143 1 0.712289 0.541948 -0.002927 11.00000 0.05859 0.03898 =
0.04657 0.03247 0.03910 0.03304
C144 1 0.728787 0.470981 -0.017532 11.00000 0.03458 0.02948 =
0.03683 0.02200 0.02630 0.01806
C145 1 0.704284 0.890131 0.989254 11.00000 0.02489 0.02492 =
0.01108 0.00571 0.00258 0.01315
C146 1 0.681595 0.806812 0.983067 11.00000 0.03440 0.02548 =
0.01860 0.00517 0.00013 0.01867
AFIX 43
H146 2 0.726490 0.786646 0.973557 11.00000 -1.20000
AFIX 0
C147 1 0.589826 0.754105 0.991464 11.00000 0.04018 0.02481 =
0.02715 0.00857 -0.00449 0.01189
AFIX 43
H147 2 0.573370 0.697786 0.987481 11.00000 -1.20000
AFIX 0
C148 1 0.521809 0.783027 1.005650 11.00000 0.02287 0.03030 =
0.02288 0.01297 0.00136 0.00341
AFIX 43
H148 2 0.460553 0.746114 1.010661 11.00000 -1.20000
AFIX 0
C149 1 0.545136 0.867328 1.012406 11.00000 0.02139 0.03510 =
0.01795 0.00931 0.00448 0.01356
AFIX 43
H149 2 0.500212 0.887202 1.022293 11.00000 -1.20000
AFIX 0
C150 1 0.635738 0.920477 1.004181 11.00000 0.02401 0.02417 =
0.00972 0.00350 0.00152 0.01406
C151 1 0.681291 1.011732 1.008329 11.00000 0.02058 0.02064 =
0.00900 0.00294 -0.00128 0.00928
C152 1 0.651265 1.073121 1.019591 11.00000 0.02687 0.02776 =
0.01448 0.00289 0.00027 0.01320
AFIX 43
H152 2 0.589133 1.061293 1.027848 11.00000 -1.20000
AFIX 0
C153 1 0.717276 1.155452 1.018378 11.00000 0.04129 0.02032 =
0.02099 0.00288 -0.00356 0.01658
AFIX 43
H153 2 0.697439 1.197610 1.026153 11.00000 -1.20000
AFIX 0
C154 1 0.808810 1.174953 1.006212 11.00000 0.03630 0.02450 =
0.01615 0.00253 -0.00839 0.00529
AFIX 43
H154 2 0.850028 1.229771 1.006203 11.00000 -1.20000
AFIX 0
C155 1 0.841996 1.112117 0.993496 11.00000 0.02786 0.02705 =
0.01248 0.00663 -0.00143 0.00708
C156 1 0.932989 1.120308 0.978076 11.00000 0.02563 0.03269 =
0.01484 0.01092 -0.00137 -0.00041
AFIX 43
H156 2 0.980320 1.172067 0.975991 11.00000 -1.20000
AFIX 0
C157 1 0.949967 1.052002 0.966472 11.00000 0.01474 0.04415 =
0.01757 0.00640 -0.00280 0.00775
AFIX 43
H157 2 1.009796 1.058853 0.956630 11.00000 -1.20000
AFIX 0
C158 1 0.881830 0.970970 0.968496 11.00000 0.02235 0.03649 =
0.01641 0.00213 -0.00046 0.01803
AFIX 43
H158 2 0.896446 0.925926 0.960073 11.00000 -1.20000
AFIX 0
C159 1 0.793679 0.960768 0.983226 11.00000 0.02474 0.02497 =
0.00950 0.00080 -0.00278 0.01422
C160 1 0.775556 1.031690 0.995134 11.00000 0.01866 0.02857 =
0.00825 0.00526 -0.00334 0.01194
C161 1 0.209683 0.395347 0.244158 11.00000 0.02782 0.02023 =
0.01270 0.00498 0.00877 0.00927
C162 1 0.188663 0.311568 0.234994 11.00000 0.03007 0.02937 =
0.01823 0.00370 0.00948 0.01330
AFIX 43
H162 2 0.234996 0.292989 0.241067 11.00000 -1.20000
AFIX 0
C163 1 0.096337 0.255993 0.216457 11.00000 0.03345 0.01968 =
0.02279 -0.00063 0.00844 0.00585
AFIX 43
H163 2 0.081383 0.199881 0.210479 11.00000 -1.20000
AFIX 0
C164 1 0.026703 0.282545 0.206800 11.00000 0.03130 0.02326 =
0.02445 0.00097 0.00430 0.00252
AFIX 43
H164 2 -0.033944 0.244435 0.194179 11.00000 -1.20000
AFIX 0
C165 1 0.047312 0.366238 0.215953 11.00000 0.02145 0.02945 =
0.01821 0.00391 0.00275 0.00753
AFIX 43
H165 2 0.000753 0.384325 0.209479 11.00000 -1.20000
AFIX 0
C166 1 0.138055 0.422297 0.234831 11.00000 0.03119 0.02414 =
0.01136 0.00614 0.00709 0.00994
C167 1 0.180828 0.513208 0.248406 11.00000 0.03160 0.02682 =
0.01149 0.00704 0.00868 0.01091
C168 1 0.148183 0.574218 0.249107 11.00000 0.02940 0.03140 =
0.01654 0.00674 0.00267 0.01427
AFIX 43
H168 2 0.085376 0.561405 0.238718 11.00000 -1.20000
AFIX 0
C169 1 0.212988 0.656240 0.266029 11.00000 0.03760 0.02386 =
0.01998 0.00768 0.00459 0.01481
AFIX 43
H169 2 0.191130 0.697296 0.266740 11.00000 -1.20000
AFIX 0
C170 1 0.306333 0.678934 0.281488 11.00000 0.03162 0.02358 =
0.01773 0.00343 0.00492 0.00310
AFIX 43
H170 2 0.346299 0.734158 0.292038 11.00000 -1.20000
AFIX 0
C171 1 0.341955 0.617778 0.281357 11.00000 0.02900 0.02701 =
0.01493 0.00788 0.00982 0.00794
C172 1 0.434475 0.628630 0.297496 11.00000 0.02863 0.02478 =
0.02010 0.00690 0.00907 0.00474
AFIX 43
H172 2 0.481090 0.681260 0.308879 11.00000 -1.20000
AFIX 0
C173 1 0.455370 0.561017 0.296308 11.00000 0.02200 0.03588 =
0.02152 0.00745 0.00614 0.00990
AFIX 43
H173 2 0.516294 0.569586 0.307341 11.00000 -1.20000
AFIX 0
C174 1 0.388481 0.479592 0.279118 11.00000 0.02811 0.02816 =
0.02493 0.01121 0.01085 0.01355
AFIX 43
H174 2 0.404885 0.435394 0.278551 11.00000 -1.20000
AFIX 0
C175 1 0.299061 0.467596 0.263358 11.00000 0.02622 0.02201 =
0.01406 0.00383 0.00609 0.00892
C176 1 0.277177 0.536214 0.264823 11.00000 0.02306 0.02185 =
0.01047 0.00561 0.00466 0.00516
F1 3 0.843897 0.933143 0.327562 11.00000 0.03317 0.04214 =
0.02510 0.00405 0.00523 0.02097
F2 3 0.666385 0.809814 0.316856 11.00000 0.04757 0.02339 =
0.02411 -0.00229 -0.00779 0.01440
F3 3 0.515151 0.836523 0.349804 11.00000 0.02049 0.02576 =
0.03668 0.01050 -0.00753 -0.00299
F4 3 0.543191 0.983439 0.397161 11.00000 0.02057 0.03807 =
0.03181 0.01136 0.00578 0.01383
F5 3 0.503496 0.103385 0.352328 11.00000 0.02358 0.05790 =
0.03432 0.01754 0.00543 0.01639
F6 3 0.410150 -0.057298 0.318415 11.00000 0.05682 0.05288 =
0.02942 0.00535 0.00184 0.03947
F7 3 0.219626 -0.138194 0.326552 11.00000 0.06490 0.02279 =
0.02685 -0.00077 -0.00973 0.00473
F8 3 0.121623 -0.058853 0.369889 11.00000 0.02225 0.04210 =
0.03113 0.01169 -0.00566 -0.00389
F9 3 0.035544 0.441864 0.083278 11.00000 0.02076 0.04487 =
0.03556 0.00541 0.00303 0.01299
F10 3 0.128429 0.596021 0.128832 11.00000 0.03915 0.03706 =
0.03842 0.01092 0.01597 0.02554
F11 3 0.306593 0.647049 0.169645 11.00000 0.04013 0.01874 =
0.03041 -0.00556 0.00562 0.00422
F12 3 0.389139 0.542051 0.168344 11.00000 0.02561 0.03173 =
0.02379 0.00031 -0.00317 0.00567
F13 3 0.041017 0.485616 0.340939 11.00000 0.01928 0.04727 =
0.02191 0.00633 0.00098 0.00764
F14 3 0.164615 0.643741 0.365054 11.00000 0.03643 0.03095 =
0.02572 0.00373 0.00406 0.01649
F15 3 0.350025 0.683667 0.392720 11.00000 0.03497 0.02061 =
0.02203 -0.00243 -0.00198 0.00163
F16 3 0.407635 0.565312 0.402548 11.00000 0.01499 0.03211 =
0.02303 0.00210 -0.00391 0.00296
F17 3 0.690758 0.580904 0.131236 11.00000 0.09278 0.11187 =
0.05515 0.05715 0.04584 0.08913
F18 3 0.856744 0.685084 0.179208 11.00000 0.16064 0.03389 =
0.03945 0.01573 0.04179 0.06012
F19 3 0.993864 0.634445 0.196325 11.00000 0.06067 0.02798 =
0.02578 -0.00496 0.00761 -0.00903
F20 3 0.964847 0.478187 0.168606 11.00000 0.02630 0.04342 =
0.02553 0.00837 0.00328 0.01561
F21 3 0.716029 0.635017 0.374520 11.00000 0.03319 0.03659 =
0.02834 0.01220 0.00626 0.02137
F22 3 0.900498 0.724679 0.406649 11.00000 0.03863 0.01935 =
0.03112 0.00719 0.00668 0.00726
F23 3 1.013261 0.649500 0.425274 11.00000 0.02172 0.03925 =
0.02822 0.00682 0.00261 0.00570
F24 3 0.940602 0.485164 0.415766 11.00000 0.03704 0.04231 =
0.02536 0.01071 0.00991 0.02826
F25 3 0.539215 0.955109 0.147256 11.00000 0.02932 0.05636 =
0.03031 0.01731 0.00973 0.02744
F26 3 0.511470 0.799119 0.119406 11.00000 0.01976 0.03991 =
0.03624 0.01964 0.00435 0.00082
F27 3 0.659908 0.763627 0.089958 11.00000 0.03764 0.02177 =
0.02885 0.00641 -0.00119 0.00835
F28 3 0.832030 0.885396 0.083545 11.00000 0.02689 0.03668 =
0.02591 0.00385 0.00499 0.01708
F29 3 0.477157 1.026345 0.087227 11.00000 0.02392 0.04858 =
0.02850 0.01498 0.00742 0.01750
F30 3 0.359868 0.866742 0.081406 11.00000 0.04443 0.03440 =
0.02416 0.00134 0.00271 0.02900
F31 3 0.175338 0.820827 0.103128 11.00000 0.03780 0.02254 =
0.02598 0.00373 -0.00385 0.00486
F32 3 0.112368 0.934792 0.136558 11.00000 0.02523 0.04237 =
0.02412 0.00813 0.00539 0.01329
I1 4 0.724197 1.150122 0.424729 11.00000 0.04350 0.02282 =
0.02096 0.00051 -0.00436 0.01675
I2 4 0.927984 1.115378 0.377682 11.00000 0.01965 0.03399 =
0.02488 0.01135 -0.00178 -0.00159
I3 4 0.184013 0.123103 0.420062 11.00000 0.03769 0.05553 =
0.02214 0.01250 0.00792 0.02923
I4 4 0.441847 0.232131 0.406826 11.00000 0.03856 0.02649 =
0.03049 0.00458 -0.01040 -0.00170
I5 4 0.324055 0.355942 0.125623 11.00000 0.03538 0.03197 =
0.02438 0.00786 0.00553 0.01869
I6 4 0.082122 0.287764 0.068918 11.00000 0.03209 0.02371 =
0.02545 -0.00048 0.00135 0.00015
I7 4 0.303516 0.372327 0.384706 11.00000 0.03496 0.02722 =
0.01904 0.00525 0.00666 0.01415
I8 4 0.052459 0.319219 0.344838 11.00000 0.02736 0.02604 =
0.02061 0.00039 0.00273 -0.00551
I9 4 0.798361 0.326189 0.111894 11.00000 0.05184 0.01825 =
0.03105 0.00173 0.01228 0.01021
I10 4 0.612333 0.395162 0.085310 11.00000 0.02275 0.09858 =
0.03315 0.03681 0.00397 0.00940
I11 4 0.741541 0.343985 0.379396 11.00000 0.05369 0.02075 =
0.02382 0.00360 0.01108 0.01434
I12 4 0.585240 0.445741 0.354735 11.00000 0.02512 0.04186 =
0.02683 0.00855 -0.00328 0.00433
I13 4 0.714708 1.124752 0.150812 11.00000 0.04971 0.03209 =
0.02165 0.00308 -0.00380 0.02420
I14 4 0.915057 1.077711 0.109040 11.00000 0.02430 0.03243 =
0.02297 0.00371 0.00006 -0.00008
I15 4 0.207940 1.127505 0.155041 11.00000 0.04527 0.04006 =
0.01881 0.00061 0.00009 0.02962
I16 4 0.458029 1.189161 0.122524 11.00000 0.03522 0.02594 =
0.02537 0.00949 -0.00498 0.00526
HKLF 4
REM 20161228b_a.res in P-1
REM R1 = 0.0449 for 28572 Fo > 4sig(Fo) and 0.0640 for all 36197 data
REM 2017 parameters refined using 1056 restraints
END
WGHT 0.0143 6.9636
REM Highest difference peak 2.457, deepest hole -3.125, 1-sigma level 0.144
Q1 1 0.6243 0.3558 0.0814 11.00000 0.05 2.46
Q2 1 0.4606 0.1895 0.3978 11.00000 0.05 1.33
Q3 1 0.1614 0.1620 0.4260 11.00000 0.05 0.96
;
_shelx_res_checksum 42580
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.411
_oxdiff_exptl_absorpt_empirical_full_min 0.752
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_20161116c
_database_code_depnum_ccdc_archive 'CCDC 1547632'
_audit_update_record
;
2017-07-20 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_audit_creation_date 2016-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common ?
_chemical_name_systematic 14DBrPB-FA
_chemical_formula_moiety 'Br2 C6 F4, C16 H10'
_chemical_formula_sum 'C22 H10 Br2 F4'
_chemical_formula_weight 510.12
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 7.2059(5)
_cell_length_b 8.3166(5)
_cell_length_c 14.8296(12)
_cell_angle_alpha 90.772(6)
_cell_angle_beta 92.296(6)
_cell_angle_gamma 91.587(5)
_cell_volume 887.57(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 2113
_cell_measurement_temperature 150.00(10)
_cell_measurement_theta_max 27.5500
_cell_measurement_theta_min 3.6880
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 4.612
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.53694
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.909
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 496
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.2
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0474
_diffrn_reflns_av_unetI/netI 0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.814
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 7250
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.814
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.906
_diffrn_reflns_theta_min 3.657
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 150.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.814
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -63.00 43.00 1.00 1.00 -- 12.76 -77.00 -90.00 106
2 \w -7.00 28.00 1.00 1.00 -- -11.04 -99.00 30.00 35
3 \w -12.00 54.00 1.00 1.00 -- 12.76 -99.00 30.00 66
4 \w -57.00 40.00 1.00 1.00 -- 12.76 -57.00 150.00 97
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0186885000
_diffrn_orient_matrix_UB_12 0.0151971000
_diffrn_orient_matrix_UB_13 0.0467078000
_diffrn_orient_matrix_UB_21 -0.0772831000
_diffrn_orient_matrix_UB_22 -0.0501430000
_diffrn_orient_matrix_UB_23 0.0103132000
_diffrn_orient_matrix_UB_31 0.0582279000
_diffrn_orient_matrix_UB_32 -0.0673479000
_diffrn_orient_matrix_UB_33 0.0019749000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2946
_reflns_number_total 4178
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.587
_refine_diff_density_min -0.659
_refine_diff_density_rms 0.133
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.985
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 253
_refine_ls_number_reflns 4178
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0786
_refine_ls_R_factor_gt 0.0489
_refine_ls_restrained_S_all 0.985
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0829
_refine_ls_wR_factor_ref 0.0980
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C15(H15), C11(H11), C14(H14), C16(H16), C20(H20), C8(H8), C22(H22), C10(H10),
C21(H21), C9(H9)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
Br1 Br 0.98650(6) 1.03117(5) 0.13282(3) 0.02861(14) Uani 1 1 d . . . . .
Br2 Br 0.97255(6) 0.36886(5) 0.36304(3) 0.02881(14) Uani 1 1 d . . . . .
F2 F 1.1264(3) 0.7009(3) 0.41930(15) 0.0276(6) Uani 1 1 d . . . . .
F3 F 0.8572(3) 0.4203(3) 0.16531(17) 0.0268(6) Uani 1 1 d . . . . .
F4 F 0.8645(3) 0.6914(3) 0.07110(16) 0.0269(6) Uani 1 1 d . . . . .
F1 F 1.1313(3) 0.9734(3) 0.32501(17) 0.0277(6) Uani 1 1 d . . . . .
C1 C 0.9952(5) 0.8389(4) 0.1965(3) 0.0173(9) Uani 1 1 d . . . . .
C3 C 1.0609(5) 0.6973(5) 0.3335(3) 0.0173(9) Uani 1 1 d . . . . .
C5 C 0.9253(5) 0.5557(4) 0.2063(3) 0.0168(9) Uani 1 1 d . . . . .
C4 C 0.9883(5) 0.5554(4) 0.2953(3) 0.0167(9) Uani 1 1 d . . . . .
C6 C 0.9290(5) 0.6953(5) 0.1571(3) 0.0174(9) Uani 1 1 d . . . . .
C13 C 0.4963(5) 0.5672(4) 0.2926(3) 0.0149(8) Uani 1 1 d . . . . .
C12 C 0.5728(5) 0.6992(4) 0.3520(3) 0.0160(9) Uani 1 1 d . . . . .
C15 C 0.3814(5) 0.3180(5) 0.2275(3) 0.0215(10) Uani 1 1 d . . . . .
H15 H 0.3560 0.2086 0.2341 0.026 Uiso 1 1 calc R . . . .
C2 C 1.0628(5) 0.8360(4) 0.2847(3) 0.0191(9) Uani 1 1 d . . . . .
C11 C 0.6379(5) 0.7008(5) 0.4417(3) 0.0203(9) Uani 1 1 d . . . . .
H11 H 0.6374 0.6072 0.4753 0.024 Uiso 1 1 calc R . . . .
C7 C 0.5770(5) 0.8424(4) 0.3011(3) 0.0150(8) Uani 1 1 d . . . . .
C19 C 0.5022(5) 0.8044(4) 0.2095(3) 0.0158(9) Uani 1 1 d . . . . .
C14 C 0.4582(5) 0.4068(4) 0.3026(3) 0.0188(9) Uani 1 1 d . . . . .
H14 H 0.4823 0.3572 0.3575 0.023 Uiso 1 1 calc R . . . .
C16 C 0.3429(5) 0.3853(5) 0.1454(3) 0.0208(9) Uani 1 1 d . . . . .
H16 H 0.2915 0.3222 0.0980 0.025 Uiso 1 1 calc R . . . .
C20 C 0.4696(5) 0.8883(5) 0.1320(3) 0.0205(9) Uani 1 1 d . . . . .
H20 H 0.4971 0.9981 0.1301 0.025 Uiso 1 1 calc R . . . .
C18 C 0.4564(5) 0.6361(4) 0.2080(3) 0.0163(9) Uani 1 1 d . . . . .
C8 C 0.6464(5) 0.9856(4) 0.3403(3) 0.0177(9) Uani 1 1 d . . . . .
H8 H 0.6514 1.0794 0.3070 0.021 Uiso 1 1 calc R . . . .
C17 C 0.3815(5) 0.5526(5) 0.1324(3) 0.0175(9) Uani 1 1 d . . . . .
C22 C 0.3508(5) 0.6435(5) 0.0532(3) 0.0210(9) Uani 1 1 d . . . . .
H22 H 0.3021 0.5935 0.0006 0.025 Uiso 1 1 calc R . . . .
C10 C 0.7040(6) 0.8467(5) 0.4798(3) 0.0242(10) Uani 1 1 d . . . . .
H10 H 0.7461 0.8500 0.5399 0.029 Uiso 1 1 calc R . . . .
C21 C 0.3930(6) 0.8047(5) 0.0545(3) 0.0246(10) Uani 1 1 d . . . . .
H21 H 0.3704 0.8625 0.0021 0.030 Uiso 1 1 calc R . . . .
C9 C 0.7083(6) 0.9861(5) 0.4305(3) 0.0244(10) Uani 1 1 d . . . . .
H9 H 0.7530 1.0816 0.4578 0.029 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0306(3) 0.0191(2) 0.0359(3) 0.0081(2) -0.0035(2) -0.00007(18)
Br2 0.0288(3) 0.0256(2) 0.0325(3) 0.0128(2) 0.0022(2) 0.00226(18)
F2 0.0329(14) 0.0385(15) 0.0105(13) -0.0023(11) -0.0079(11) -0.0012(11)
F3 0.0311(14) 0.0168(12) 0.0315(15) -0.0098(11) -0.0067(12) -0.0041(10)
F4 0.0357(15) 0.0288(13) 0.0152(14) -0.0048(11) -0.0084(11) -0.0017(11)
F1 0.0309(14) 0.0222(13) 0.0286(15) -0.0125(11) -0.0056(12) -0.0076(10)
C1 0.018(2) 0.018(2) 0.017(2) 0.0006(18) -0.0021(17) 0.0044(16)
C3 0.017(2) 0.027(2) 0.007(2) -0.0033(18) -0.0005(16) 0.0011(17)
C5 0.019(2) 0.014(2) 0.016(2) -0.0052(18) -0.0026(17) -0.0014(16)
C4 0.021(2) 0.016(2) 0.014(2) -0.0014(18) 0.0011(17) 0.0006(16)
C6 0.017(2) 0.024(2) 0.011(2) -0.0071(18) -0.0030(17) 0.0007(16)
C13 0.014(2) 0.020(2) 0.011(2) -0.0037(18) 0.0011(16) 0.0026(16)
C12 0.015(2) 0.018(2) 0.015(2) -0.0009(18) 0.0009(17) 0.0026(15)
C15 0.022(2) 0.013(2) 0.030(3) -0.0052(19) 0.005(2) -0.0012(16)
C2 0.019(2) 0.016(2) 0.021(2) -0.0102(19) 0.0001(18) -0.0032(16)
C11 0.024(2) 0.019(2) 0.018(2) -0.0042(19) -0.0019(19) 0.0024(17)
C7 0.012(2) 0.018(2) 0.015(2) -0.0056(17) 0.0016(17) 0.0006(15)
C19 0.012(2) 0.017(2) 0.018(2) -0.0019(18) 0.0021(17) -0.0027(15)
C14 0.024(2) 0.018(2) 0.015(2) 0.0011(18) -0.0005(18) 0.0003(17)
C16 0.018(2) 0.021(2) 0.022(2) -0.0125(19) 0.0005(18) -0.0048(17)
C20 0.025(2) 0.019(2) 0.018(2) 0.0015(19) 0.0011(19) 0.0028(17)
C18 0.013(2) 0.018(2) 0.018(2) -0.0019(18) 0.0017(17) 0.0015(15)
C8 0.022(2) 0.0140(19) 0.017(2) -0.0002(18) -0.0004(18) 0.0020(16)
C17 0.017(2) 0.024(2) 0.011(2) -0.0044(18) 0.0017(17) -0.0005(17)
C22 0.019(2) 0.033(2) 0.011(2) -0.0047(19) -0.0012(17) -0.0013(18)
C10 0.024(2) 0.031(2) 0.018(2) -0.008(2) -0.0031(19) 0.0020(19)
C21 0.025(2) 0.035(3) 0.014(2) 0.006(2) -0.0011(19) 0.0057(19)
C9 0.028(2) 0.018(2) 0.026(3) -0.012(2) -0.003(2) -0.0003(18)
_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
Br1 C1 1.869(4) . ?
Br2 C4 1.863(4) . ?
F2 C3 1.339(4) . ?
F3 C5 1.343(4) . ?
F4 C6 1.339(4) . ?
F1 C2 1.354(4) . ?
C1 C6 1.386(5) . ?
C1 C2 1.378(5) . ?
C3 C4 1.383(5) . ?
C3 C2 1.370(5) . ?
C5 C4 1.378(5) . ?
C5 C6 1.380(5) . ?
C13 C12 1.478(5) . ?
C13 C14 1.366(5) . ?
C13 C18 1.409(5) . ?
C12 C11 1.394(5) . ?
C12 C7 1.418(5) . ?
C15 H15 0.9300 . ?
C15 C14 1.414(6) . ?
C15 C16 1.369(6) . ?
C11 H11 0.9300 . ?
C11 C10 1.394(5) . ?
C7 C19 1.468(5) . ?
C7 C8 1.391(5) . ?
C19 C20 1.368(5) . ?
C19 C18 1.429(5) . ?
C14 H14 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.428(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.419(6) . ?
C18 C17 1.393(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.392(6) . ?
C17 C22 1.418(6) . ?
C22 H22 0.9300 . ?
C22 C21 1.367(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.380(6) . ?
C21 H21 0.9300 . ?
C9 H9 0.9300 . ?
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
C6 C1 Br1 120.9(3) . . ?
C2 C1 Br1 121.1(3) . . ?
C2 C1 C6 117.9(4) . . ?
F2 C3 C4 120.1(4) . . ?
F2 C3 C2 119.5(4) . . ?
C2 C3 C4 120.4(4) . . ?
F3 C5 C4 120.9(3) . . ?
F3 C5 C6 118.1(4) . . ?
C4 C5 C6 120.9(4) . . ?
C3 C4 Br2 120.8(3) . . ?
C5 C4 Br2 120.7(3) . . ?
C5 C4 C3 118.5(4) . . ?
F4 C6 C1 120.2(4) . . ?
F4 C6 C5 119.3(3) . . ?
C5 C6 C1 120.5(4) . . ?
C14 C13 C12 135.4(4) . . ?
C14 C13 C18 118.4(4) . . ?
C18 C13 C12 106.3(3) . . ?
C11 C12 C13 131.5(4) . . ?
C11 C12 C7 120.3(4) . . ?
C7 C12 C13 108.2(3) . . ?
C14 C15 H15 118.5 . . ?
C16 C15 H15 118.5 . . ?
C16 C15 C14 123.1(4) . . ?
F1 C2 C1 119.7(3) . . ?
F1 C2 C3 118.7(4) . . ?
C3 C2 C1 121.6(4) . . ?
C12 C11 H11 120.9 . . ?
C12 C11 C10 118.2(4) . . ?
C10 C11 H11 120.9 . . ?
C12 C7 C19 108.3(3) . . ?
C8 C7 C12 120.3(4) . . ?
C8 C7 C19 131.4(4) . . ?
C20 C19 C7 136.1(4) . . ?
C20 C19 C18 117.9(4) . . ?
C18 C19 C7 106.1(3) . . ?
C13 C14 C15 118.4(4) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C17 120.0(4) . . ?
C17 C16 H16 120.0 . . ?
C19 C20 H20 120.6 . . ?
C19 C20 C21 118.8(4) . . ?
C21 C20 H20 120.6 . . ?
C13 C18 C19 111.2(3) . . ?
C17 C18 C13 124.9(4) . . ?
C17 C18 C19 123.9(4) . . ?
C7 C8 H8 120.6 . . ?
C7 C8 C9 118.8(4) . . ?
C9 C8 H8 120.6 . . ?
C18 C17 C16 115.2(4) . . ?
C18 C17 C22 116.6(4) . . ?
C22 C17 C16 128.2(4) . . ?
C17 C22 H22 120.1 . . ?
C21 C22 C17 119.7(4) . . ?
C21 C22 H22 120.1 . . ?
C11 C10 H10 119.2 . . ?
C9 C10 C11 121.7(4) . . ?
C9 C10 H10 119.2 . . ?
C20 C21 H21 118.4 . . ?
C22 C21 C20 123.1(4) . . ?
C22 C21 H21 118.4 . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.7(4) . . ?
C10 C9 H9 119.6 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C1 C6 F4 2.7(5) . . . . ?
Br1 C1 C6 C5 -176.0(3) . . . . ?
Br1 C1 C2 F1 -2.8(5) . . . . ?
Br1 C1 C2 C3 176.6(3) . . . . ?
F2 C3 C4 Br2 2.1(5) . . . . ?
F2 C3 C4 C5 -178.9(3) . . . . ?
F2 C3 C2 F1 0.0(5) . . . . ?
F2 C3 C2 C1 -179.3(3) . . . . ?
F3 C5 C4 Br2 -2.4(5) . . . . ?
F3 C5 C4 C3 178.5(3) . . . . ?
F3 C5 C6 F4 0.3(5) . . . . ?
F3 C5 C6 C1 179.0(3) . . . . ?
C4 C3 C2 F1 178.6(3) . . . . ?
C4 C3 C2 C1 -0.8(6) . . . . ?
C4 C5 C6 F4 -179.2(3) . . . . ?
C4 C5 C6 C1 -0.5(6) . . . . ?
C6 C1 C2 F1 179.0(3) . . . . ?
C6 C1 C2 C3 -1.7(6) . . . . ?
C6 C5 C4 Br2 177.0(3) . . . . ?
C6 C5 C4 C3 -2.0(6) . . . . ?
C13 C12 C11 C10 179.6(4) . . . . ?
C13 C12 C7 C19 0.5(4) . . . . ?
C13 C12 C7 C8 -178.9(3) . . . . ?
C13 C18 C17 C16 0.7(6) . . . . ?
C13 C18 C17 C22 179.8(4) . . . . ?
C12 C13 C14 C15 179.5(4) . . . . ?
C12 C13 C18 C19 -0.2(4) . . . . ?
C12 C13 C18 C17 -179.9(4) . . . . ?
C12 C11 C10 C9 -1.0(6) . . . . ?
C12 C7 C19 C20 179.3(4) . . . . ?
C12 C7 C19 C18 -0.6(4) . . . . ?
C12 C7 C8 C9 -1.1(5) . . . . ?
C15 C16 C17 C18 -0.6(5) . . . . ?
C15 C16 C17 C22 -179.7(4) . . . . ?
C2 C1 C6 F4 -179.0(3) . . . . ?
C2 C1 C6 C5 2.3(6) . . . . ?
C2 C3 C4 Br2 -176.4(3) . . . . ?
C2 C3 C4 C5 2.6(6) . . . . ?
C11 C12 C7 C19 179.4(3) . . . . ?
C11 C12 C7 C8 0.1(6) . . . . ?
C11 C10 C9 C8 -0.1(6) . . . . ?
C7 C12 C11 C10 1.0(6) . . . . ?
C7 C19 C20 C21 179.9(4) . . . . ?
C7 C19 C18 C13 0.5(4) . . . . ?
C7 C19 C18 C17 -179.8(4) . . . . ?
C7 C8 C9 C10 1.1(6) . . . . ?
C19 C7 C8 C9 179.7(4) . . . . ?
C19 C20 C21 C22 -0.4(6) . . . . ?
C19 C18 C17 C16 -179.1(3) . . . . ?
C19 C18 C17 C22 0.1(6) . . . . ?
C14 C13 C12 C11 1.7(7) . . . . ?
C14 C13 C12 C7 -179.5(4) . . . . ?
C14 C13 C18 C19 179.3(3) . . . . ?
C14 C13 C18 C17 -0.5(6) . . . . ?
C14 C15 C16 C17 0.5(6) . . . . ?
C16 C15 C14 C13 -0.2(6) . . . . ?
C16 C17 C22 C21 178.4(4) . . . . ?
C20 C19 C18 C13 -179.4(3) . . . . ?
C20 C19 C18 C17 0.3(6) . . . . ?
C18 C13 C12 C11 -179.0(4) . . . . ?
C18 C13 C12 C7 -0.2(4) . . . . ?
C18 C13 C14 C15 0.2(5) . . . . ?
C18 C19 C20 C21 -0.2(5) . . . . ?
C18 C17 C22 C21 -0.6(6) . . . . ?
C8 C7 C19 C20 -1.4(8) . . . . ?
C8 C7 C19 C18 178.7(4) . . . . ?
C17 C22 C21 C20 0.8(6) . . . . ?
_shelx_res_file
;
20161116c.res created by SHELXL-2014/7
TITL 20161116c_a.res in P-1
REM Old TITL 20161116c in P-1 #2
REM SHELXT solution in P-1
REM R1 0.125, Rweak 0.009, Alpha 0.072, Orientation as input
REM Formula found by SHELXT: C8 O4 Br2
CELL 0.71073 7.205905 8.316621 14.829576 90.7725 92.2959 91.5872
ZERR 2 0.000482 0.000522 0.001164 0.0057 0.0059 0.0053
LATT 1
SFAC C H Br F
UNIT 44 20 4 8
L.S. 5
PLAN 5
BOND $H
MORE -1
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.019700
FVAR 0.46349
BR1 3 0.986502 1.031173 0.132825 11.00000 0.03058 0.01908 =
0.03594 0.00807 -0.00348 -0.00007
BR2 3 0.972546 0.368858 0.363037 11.00000 0.02882 0.02563 =
0.03248 0.01280 0.00224 0.00226
F2 4 1.126359 0.700857 0.419299 11.00000 0.03291 0.03855 =
0.01055 -0.00234 -0.00788 -0.00123
F3 4 0.857228 0.420301 0.165311 11.00000 0.03111 0.01676 =
0.03147 -0.00980 -0.00668 -0.00407
F4 4 0.864454 0.691449 0.071101 11.00000 0.03569 0.02882 =
0.01519 -0.00476 -0.00839 -0.00166
F1 4 1.131301 0.973390 0.325014 11.00000 0.03086 0.02221 =
0.02858 -0.01253 -0.00563 -0.00755
C1 1 0.995184 0.838861 0.196452 11.00000 0.01761 0.01758 =
0.01661 0.00064 -0.00208 0.00435
C3 1 1.060931 0.697325 0.333483 11.00000 0.01712 0.02750 =
0.00716 -0.00334 -0.00049 0.00114
C5 1 0.925314 0.555660 0.206316 11.00000 0.01929 0.01444 =
0.01627 -0.00519 -0.00260 -0.00140
C4 1 0.988346 0.555402 0.295307 11.00000 0.02075 0.01578 =
0.01361 -0.00140 0.00109 0.00064
C6 1 0.928992 0.695283 0.157063 11.00000 0.01673 0.02372 =
0.01128 -0.00712 -0.00299 0.00074
C13 1 0.496252 0.567215 0.292623 11.00000 0.01381 0.02020 =
0.01071 -0.00370 0.00113 0.00262
C12 1 0.572767 0.699215 0.351955 11.00000 0.01504 0.01763 =
0.01532 -0.00086 0.00092 0.00260
C15 1 0.381448 0.317963 0.227453 11.00000 0.02228 0.01253 =
0.02961 -0.00521 0.00486 -0.00121
AFIX 43
H15 2 0.355952 0.208633 0.234121 11.00000 -1.20000
AFIX 0
C2 1 1.062794 0.836023 0.284677 11.00000 0.01908 0.01630 =
0.02147 -0.01015 0.00010 -0.00323
C11 1 0.637931 0.700846 0.441731 11.00000 0.02393 0.01885 =
0.01775 -0.00417 -0.00188 0.00244
AFIX 43
H11 2 0.637384 0.607234 0.475334 11.00000 -1.20000
AFIX 0
C7 1 0.576999 0.842361 0.301069 11.00000 0.01230 0.01774 =
0.01486 -0.00561 0.00155 0.00057
C19 1 0.502239 0.804420 0.209459 11.00000 0.01169 0.01717 =
0.01829 -0.00192 0.00214 -0.00272
C14 1 0.458240 0.406782 0.302609 11.00000 0.02350 0.01808 =
0.01472 0.00107 -0.00050 0.00030
AFIX 43
H14 2 0.482278 0.357154 0.357509 11.00000 -1.20000
AFIX 0
C16 1 0.342887 0.385349 0.145358 11.00000 0.01779 0.02143 =
0.02247 -0.01253 0.00054 -0.00475
AFIX 43
H16 2 0.291532 0.322182 0.097986 11.00000 -1.20000
AFIX 0
C20 1 0.469590 0.888282 0.132003 11.00000 0.02462 0.01869 =
0.01822 0.00147 0.00107 0.00284
AFIX 43
H20 2 0.497104 0.998073 0.130136 11.00000 -1.20000
AFIX 0
C18 1 0.456413 0.636138 0.208001 11.00000 0.01296 0.01821 =
0.01789 -0.00188 0.00168 0.00152
C8 1 0.646402 0.985644 0.340341 11.00000 0.02210 0.01400 =
0.01701 -0.00015 -0.00044 0.00198
AFIX 43
H8 2 0.651395 1.079442 0.306977 11.00000 -1.20000
AFIX 0
C17 1 0.381480 0.552615 0.132418 11.00000 0.01681 0.02432 =
0.01130 -0.00445 0.00172 -0.00050
C22 1 0.350772 0.643471 0.053218 11.00000 0.01895 0.03275 =
0.01103 -0.00471 -0.00118 -0.00127
AFIX 43
H22 2 0.302138 0.593518 0.000629 11.00000 -1.20000
AFIX 0
C10 1 0.703952 0.846653 0.479777 11.00000 0.02380 0.03057 =
0.01776 -0.00786 -0.00306 0.00203
AFIX 43
H10 2 0.746146 0.849981 0.539884 11.00000 -1.20000
AFIX 0
C21 1 0.392957 0.804743 0.054516 11.00000 0.02498 0.03521 =
0.01394 0.00593 -0.00111 0.00566
AFIX 43
H21 2 0.370374 0.862493 0.002131 11.00000 -1.20000
AFIX 0
C9 1 0.708274 0.986143 0.430506 11.00000 0.02840 0.01844 =
0.02566 -0.01155 -0.00295 -0.00032
AFIX 43
H9 2 0.753022 1.081589 0.457826 11.00000 -1.20000
AFIX 0
HKLF 4
REM 20161116c_a.res in P-1
REM R1 = 0.0489 for 2946 Fo > 4sig(Fo) and 0.0786 for all 4178 data
REM 253 parameters refined using 0 restraints
END
WGHT 0.0197 0.0000
REM Highest difference peak 0.587, deepest hole -0.659, 1-sigma level 0.133
Q1 1 0.9134 1.1409 0.1390 11.00000 0.05 0.59
Q2 1 0.8929 0.4626 0.3623 11.00000 0.05 0.58
Q3 1 0.9169 1.0934 0.2579 11.00000 0.05 0.56
Q4 1 0.8566 1.0034 0.1353 11.00000 0.05 0.52
Q5 1 0.9409 0.2013 0.2750 11.00000 0.05 0.48
;
_shelx_res_checksum 43079
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.365
_oxdiff_exptl_absorpt_empirical_full_min 0.761
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_20161213b
_database_code_depnum_ccdc_archive 'CCDC 1547631'
_audit_update_record
;
2017-07-20 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_audit_creation_date 2016-12-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common ?
_chemical_name_systematic 13DBrPB
_chemical_formula_moiety 'Br2 C6 F4, C16 H10'
_chemical_formula_sum 'C22 H10 Br2 F4'
_chemical_formula_weight 510.12
_chemical_melting_point ?
_chemical_oxdiff_formula c1h1f1Br1
_chemical_oxdiff_usercomment Eu
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'
_cell_length_a 6.8502(7)
_cell_length_b 8.0650(7)
_cell_length_c 17.0969(16)
_cell_angle_alpha 97.180(8)
_cell_angle_beta 100.583(8)
_cell_angle_gamma 100.330(8)
_cell_volume 901.17(15)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 1976
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 25.9480
_cell_measurement_theta_min 3.4930
_exptl_absorpt_coefficient_mu 4.542
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.28618
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.880
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description cube
_exptl_crystal_F_000 496
_exptl_crystal_size_max 0.6
_exptl_crystal_size_mid 0.6
_exptl_crystal_size_min 0.25
_exptl_special_details
;
?
;
_diffrn_reflns_av_R_equivalents 0.0575
_diffrn_reflns_av_unetI/netI 0.0878
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 6885
_diffrn_reflns_theta_full 25.35
_diffrn_reflns_theta_max 25.35
_diffrn_reflns_theta_min 3.27
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.8270
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -9.00 81.00 1.00 2.00 -- 12.76 37.00 -60.00 90
2 \w -16.00 30.00 1.00 2.00 -- -11.04 -99.00 120.00 46
3 \w -32.00 49.00 1.00 2.00 -- 12.76 -88.00 82.00 81
4 \w 67.00 95.00 1.00 2.00 -- 12.76-178.00 90.00 28
5 \w -49.00 50.00 1.00 2.00 -- 12.76 0.00 90.00 99
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0538840000
_diffrn_orient_matrix_UB_12 -0.0701078000
_diffrn_orient_matrix_UB_13 -0.0300761000
_diffrn_orient_matrix_UB_21 -0.0717163000
_diffrn_orient_matrix_UB_22 -0.0201785000
_diffrn_orient_matrix_UB_23 0.0242706000
_diffrn_orient_matrix_UB_31 -0.0595633000
_diffrn_orient_matrix_UB_32 0.0537447000
_diffrn_orient_matrix_UB_33 -0.0183419000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_reflns_number_gt 2448
_reflns_number_total 3299
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_threshold_expression >2sigma(I)
_computing_cell_refinement 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max 0.491
_refine_diff_density_min -0.670
_refine_diff_density_rms 0.123
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.065
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 253
_refine_ls_number_reflns 3299
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0808
_refine_ls_R_factor_gt 0.0542
_refine_ls_restrained_S_all 1.065
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.2056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1092
_refine_ls_wR_factor_ref 0.1237
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C26(H26), C19(H19), C27(H27), C22(H22), C20(H20), C28(H28), C14(H14),
C24(H24), C25(H25), C21(H21)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Br7 Br 0.38192(9) 0.98183(9) 0.89749(3) 0.0354(2) Uani 1 d . . .
Br8 Br 0.28471(10) 0.93638(10) 0.55950(4) 0.0449(2) Uani 1 d . . .
F12 F 0.3738(5) 1.0970(4) 0.73532(19) 0.0327(8) Uani 1 d . . .
F11 F 0.1841(5) 0.5580(5) 0.57056(18) 0.0399(9) Uani 1 d . . .
F9 F 0.2586(5) 0.5950(5) 0.84889(19) 0.0382(9) Uani 1 d . . .
F10 F 0.1771(5) 0.4061(4) 0.7012(2) 0.0415(9) Uani 1 d . . .
C2 C 0.3257(7) 0.9265(7) 0.7272(3) 0.0218(13) Uani 1 d . . .
C1 C 0.3192(8) 0.8481(7) 0.7940(3) 0.0217(12) Uani 1 d . . .
C16 C 0.2256(8) 0.2575(7) 0.2615(3) 0.0233(13) Uani 1 d . . .
C26 C 0.1261(8) -0.0188(7) 0.1799(3) 0.0247(13) Uani 1 d . . .
H26 H 0.0939 -0.0904 0.1303 0.030 Uiso 1 calc . . R
C4 C 0.2317(8) 0.6563(8) 0.6433(3) 0.0258(13) Uani 1 d . . .
C23 C 0.1820(8) 0.1553(7) 0.1849(3) 0.0242(13) Uani 1 d . . .
C15 C 0.2167(8) 0.1945(7) 0.3333(3) 0.0233(13) Uani 1 d . . .
C19 C 0.3069(8) 0.5767(7) 0.1284(3) 0.0237(13) Uani 1 d . . .
H19 H 0.3485 0.6881 0.1562 0.028 Uiso 1 calc . . R
C13 C 0.2078(7) 0.2740(7) 0.1270(3) 0.0216(13) Uani 1 d . . .
C27 C 0.1187(8) -0.0871(8) 0.2524(3) 0.0291(14) Uani 1 d . . .
H27 H 0.0834 -0.2049 0.2495 0.035 Uiso 1 calc . . R
C17 C 0.2788(8) 0.4329(7) 0.2558(3) 0.0232(13) Uani 1 d . . .
C18 C 0.2693(8) 0.4422(7) 0.1696(3) 0.0208(12) Uani 1 d . . .
C6 C 0.2684(8) 0.6733(7) 0.7846(3) 0.0221(13) Uani 1 d . . .
C22 C 0.1847(7) 0.2434(7) 0.0435(3) 0.0216(12) Uani 1 d . . .
H22 H 0.1444 0.1325 0.0152 0.026 Uiso 1 calc . . R
C20 C 0.2822(9) 0.5445(8) 0.0452(3) 0.0308(14) Uani 1 d . . .
H20 H 0.3062 0.6354 0.0173 0.037 Uiso 1 calc . . R
C28 C 0.1615(8) 0.0146(7) 0.3260(3) 0.0274(13) Uani 1 d . . .
H28 H 0.1543 -0.0350 0.3719 0.033 Uiso 1 calc . . R
C14 C 0.2678(8) 0.3192(9) 0.4038(3) 0.0303(15) Uani 1 d . . .
H14 H 0.2630 0.2852 0.4536 0.036 Uiso 1 calc . . R
C24 C 0.3310(8) 0.5495(8) 0.3259(3) 0.0284(14) Uani 1 d . . .
H24 H 0.3700 0.6656 0.3247 0.034 Uiso 1 calc . . R
C25 C 0.3242(8) 0.4893(8) 0.3999(3) 0.0308(15) Uani 1 d . . .
H25 H 0.3593 0.5678 0.4474 0.037 Uiso 1 calc . . R
C21 C 0.2225(8) 0.3801(8) 0.0030(3) 0.0276(13) Uani 1 d . . .
H21 H 0.2077 0.3611 -0.0527 0.033 Uiso 1 calc . . R
C3 C 0.2809(8) 0.8313(8) 0.6506(3) 0.0250(13) Uani 1 d . . .
C5 C 0.2241(8) 0.5769(8) 0.7098(3) 0.0281(14) Uani 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br7 0.0323(4) 0.0511(5) 0.0225(3) -0.0052(3) 0.0047(2) 0.0167(3)
Br8 0.0513(4) 0.0619(5) 0.0296(4) 0.0240(3) 0.0118(3) 0.0180(4)
F12 0.0396(19) 0.0176(19) 0.043(2) 0.0073(16) 0.0105(16) 0.0069(16)
F11 0.039(2) 0.047(2) 0.0276(19) -0.0152(17) 0.0079(15) 0.0068(19)
F9 0.042(2) 0.045(2) 0.038(2) 0.0237(18) 0.0192(16) 0.0156(19)
F10 0.043(2) 0.017(2) 0.068(3) 0.0020(18) 0.0233(18) 0.0054(17)
C2 0.018(3) 0.022(3) 0.026(3) 0.004(3) 0.004(2) 0.008(3)
C1 0.019(3) 0.026(3) 0.014(3) -0.011(2) -0.002(2) 0.005(3)
C16 0.021(3) 0.029(4) 0.025(3) 0.008(3) 0.008(2) 0.015(3)
C26 0.025(3) 0.021(3) 0.032(3) 0.005(3) 0.009(2) 0.010(3)
C4 0.023(3) 0.031(4) 0.022(3) -0.008(3) 0.007(2) 0.006(3)
C23 0.027(3) 0.026(4) 0.026(3) 0.007(3) 0.010(2) 0.014(3)
C15 0.018(3) 0.026(3) 0.029(3) 0.007(3) 0.007(2) 0.009(3)
C19 0.023(3) 0.019(3) 0.028(3) 0.000(3) 0.006(2) 0.006(3)
C13 0.019(3) 0.027(3) 0.024(3) 0.006(3) 0.008(2) 0.014(3)
C27 0.023(3) 0.026(4) 0.043(4) 0.012(3) 0.009(3) 0.011(3)
C17 0.022(3) 0.029(4) 0.025(3) 0.008(3) 0.011(2) 0.015(3)
C18 0.022(3) 0.021(3) 0.022(3) 0.000(2) 0.006(2) 0.012(3)
C6 0.020(3) 0.028(4) 0.022(3) 0.006(3) 0.008(2) 0.009(3)
C22 0.022(3) 0.015(3) 0.028(3) 0.000(2) 0.006(2) 0.005(2)
C20 0.037(3) 0.029(4) 0.034(3) 0.014(3) 0.014(3) 0.013(3)
C28 0.035(3) 0.025(4) 0.024(3) 0.009(3) 0.009(3) 0.005(3)
C14 0.023(3) 0.049(5) 0.024(3) 0.011(3) 0.010(2) 0.009(3)
C24 0.025(3) 0.032(4) 0.033(3) 0.005(3) 0.010(3) 0.015(3)
C25 0.026(3) 0.039(4) 0.024(3) -0.007(3) 0.002(2) 0.007(3)
C21 0.035(3) 0.028(4) 0.020(3) 0.004(3) 0.007(2) 0.004(3)
C3 0.026(3) 0.032(4) 0.024(3) 0.012(3) 0.008(2) 0.014(3)
C5 0.022(3) 0.022(3) 0.041(4) 0.001(3) 0.009(3) 0.006(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
Br7 C1 1.886(5) . ?
Br8 C3 1.866(5) . ?
F12 C2 1.338(6) . ?
F11 C4 1.339(6) . ?
F9 C6 1.340(6) . ?
F10 C5 1.340(7) . ?
C2 C1 1.376(7) . ?
C2 C3 1.384(7) . ?
C1 C6 1.372(8) . ?
C16 C23 1.408(7) . ?
C16 C15 1.393(7) . ?
C16 C17 1.416(8) . ?
C26 H26 0.9300 . ?
C26 C23 1.375(8) . ?
C26 C27 1.422(7) . ?
C4 C3 1.375(8) . ?
C4 C5 1.376(8) . ?
C23 C13 1.472(7) . ?
C15 C28 1.416(8) . ?
C15 C14 1.416(8) . ?
C19 H19 0.9300 . ?
C19 C18 1.377(7) . ?
C19 C20 1.388(7) . ?
C13 C18 1.409(8) . ?
C13 C22 1.393(7) . ?
C27 H27 0.9300 . ?
C27 C28 1.364(8) . ?
C17 C18 1.475(7) . ?
C17 C24 1.374(7) . ?
C6 C5 1.363(8) . ?
C22 H22 0.9300 . ?
C22 C21 1.383(7) . ?
C20 H20 0.9300 . ?
C20 C21 1.379(8) . ?
C28 H28 0.9300 . ?
C14 H14 0.9300 . ?
C14 C25 1.370(9) . ?
C24 H24 0.9300 . ?
C24 C25 1.416(7) . ?
C25 H25 0.9300 . ?
C21 H21 0.9300 . ?
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
F12 C2 C1 120.3(5) . . ?
F12 C2 C3 118.8(5) . . ?
C1 C2 C3 120.9(5) . . ?
C2 C1 Br7 119.7(4) . . ?
C6 C1 Br7 120.6(4) . . ?
C6 C1 C2 119.6(5) . . ?
C23 C16 C17 111.0(5) . . ?
C15 C16 C23 124.5(5) . . ?
C15 C16 C17 124.5(5) . . ?
C23 C26 H26 120.7 . . ?
C23 C26 C27 118.5(5) . . ?
C27 C26 H26 120.7 . . ?
F11 C4 C3 120.6(5) . . ?
F11 C4 C5 118.0(5) . . ?
C3 C4 C5 121.4(5) . . ?
C16 C23 C13 106.1(5) . . ?
C26 C23 C16 118.2(5) . . ?
C26 C23 C13 135.7(5) . . ?
C16 C15 C28 115.7(5) . . ?
C16 C15 C14 115.5(5) . . ?
C14 C15 C28 128.8(5) . . ?
C18 C19 H19 120.3 . . ?
C18 C19 C20 119.4(5) . . ?
C20 C19 H19 120.3 . . ?
C18 C13 C23 108.9(5) . . ?
C22 C13 C23 130.9(5) . . ?
C22 C13 C18 120.2(5) . . ?
C26 C27 H27 118.9 . . ?
C28 C27 C26 122.2(6) . . ?
C28 C27 H27 118.9 . . ?
C16 C17 C18 106.6(5) . . ?
C24 C17 C16 118.2(5) . . ?
C24 C17 C18 135.2(6) . . ?
C19 C18 C13 119.8(5) . . ?
C19 C18 C17 132.8(5) . . ?
C13 C18 C17 107.4(5) . . ?
F9 C6 C1 120.4(5) . . ?
F9 C6 C5 119.1(5) . . ?
C5 C6 C1 120.5(5) . . ?
C13 C22 H22 120.4 . . ?
C21 C22 C13 119.2(5) . . ?
C21 C22 H22 120.4 . . ?
C19 C20 H20 119.4 . . ?
C21 C20 C19 121.2(5) . . ?
C21 C20 H20 119.4 . . ?
C15 C28 H28 119.6 . . ?
C27 C28 C15 120.9(5) . . ?
C27 C28 H28 119.6 . . ?
C15 C14 H14 119.5 . . ?
C25 C14 C15 121.0(5) . . ?
C25 C14 H14 119.5 . . ?
C17 C24 H24 120.7 . . ?
C17 C24 C25 118.6(6) . . ?
C25 C24 H24 120.7 . . ?
C14 C25 C24 122.3(6) . . ?
C14 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?
C22 C21 H21 119.9 . . ?
C20 C21 C22 120.2(5) . . ?
C20 C21 H21 119.9 . . ?
C2 C3 Br8 121.2(5) . . ?
C4 C3 Br8 120.7(4) . . ?
C4 C3 C2 118.1(5) . . ?
F10 C5 C4 120.4(5) . . ?
F10 C5 C6 120.1(5) . . ?
C6 C5 C4 119.5(6) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br7 C1 C6 F9 1.4(7) . . . . ?
Br7 C1 C6 C5 -179.7(4) . . . . ?
F12 C2 C1 Br7 -0.8(6) . . . . ?
F12 C2 C1 C6 179.6(4) . . . . ?
F12 C2 C3 Br8 -0.5(6) . . . . ?
F12 C2 C3 C4 -180.0(5) . . . . ?
F11 C4 C3 Br8 -0.5(7) . . . . ?
F11 C4 C3 C2 179.0(4) . . . . ?
F11 C4 C5 F10 2.3(7) . . . . ?
F11 C4 C5 C6 -179.0(4) . . . . ?
F9 C6 C5 F10 -1.9(7) . . . . ?
F9 C6 C5 C4 179.3(4) . . . . ?
C2 C1 C6 F9 -179.0(4) . . . . ?
C2 C1 C6 C5 -0.1(8) . . . . ?
C1 C2 C3 Br8 178.9(4) . . . . ?
C1 C2 C3 C4 -0.6(7) . . . . ?
C1 C6 C5 F10 179.1(5) . . . . ?
C1 C6 C5 C4 0.4(8) . . . . ?
C16 C23 C13 C18 1.1(5) . . . . ?
C16 C23 C13 C22 179.9(5) . . . . ?
C16 C15 C28 C27 -0.6(7) . . . . ?
C16 C15 C14 C25 -0.8(7) . . . . ?
C16 C17 C18 C19 -179.2(5) . . . . ?
C16 C17 C18 C13 1.1(5) . . . . ?
C16 C17 C24 C25 -1.6(7) . . . . ?
C26 C23 C13 C18 179.9(6) . . . . ?
C26 C23 C13 C22 -1.2(10) . . . . ?
C26 C27 C28 C15 -0.3(8) . . . . ?
C23 C16 C15 C28 0.7(7) . . . . ?
C23 C16 C15 C14 179.6(5) . . . . ?
C23 C16 C17 C18 -0.4(6) . . . . ?
C23 C16 C17 C24 -178.3(4) . . . . ?
C23 C26 C27 C28 1.2(8) . . . . ?
C23 C13 C18 C19 178.9(4) . . . . ?
C23 C13 C18 C17 -1.3(5) . . . . ?
C23 C13 C22 C21 -178.8(5) . . . . ?
C15 C16 C23 C26 0.2(8) . . . . ?
C15 C16 C23 C13 179.2(4) . . . . ?
C15 C16 C17 C18 180.0(5) . . . . ?
C15 C16 C17 C24 2.0(7) . . . . ?
C15 C14 C25 C24 1.2(8) . . . . ?
C19 C20 C21 C22 0.4(8) . . . . ?
C13 C22 C21 C20 -0.1(8) . . . . ?
C27 C26 C23 C16 -1.1(7) . . . . ?
C27 C26 C23 C13 -179.8(5) . . . . ?
C17 C16 C23 C26 -179.5(5) . . . . ?
C17 C16 C23 C13 -0.4(6) . . . . ?
C17 C16 C15 C28 -179.6(5) . . . . ?
C17 C16 C15 C14 -0.8(7) . . . . ?
C17 C24 C25 C14 0.1(8) . . . . ?
C18 C19 C20 C21 -0.6(8) . . . . ?
C18 C13 C22 C21 -0.1(7) . . . . ?
C18 C17 C24 C25 -178.8(5) . . . . ?
C22 C13 C18 C19 -0.1(7) . . . . ?
C22 C13 C18 C17 179.7(4) . . . . ?
C20 C19 C18 C13 0.5(7) . . . . ?
C20 C19 C18 C17 -179.3(5) . . . . ?
C28 C15 C14 C25 177.9(5) . . . . ?
C14 C15 C28 C27 -179.3(5) . . . . ?
C24 C17 C18 C19 -1.7(10) . . . . ?
C24 C17 C18 C13 178.5(5) . . . . ?
C3 C2 C1 Br7 179.8(4) . . . . ?
C3 C2 C1 C6 0.2(7) . . . . ?
C3 C4 C5 F10 -179.5(5) . . . . ?
C3 C4 C5 C6 -0.8(8) . . . . ?
C5 C4 C3 Br8 -178.7(4) . . . . ?
C5 C4 C3 C2 0.9(8) . . . . ?
_iucr_refine_instructions_details
;
TITL 20161213b_a.res in P-1
REM Old TITL 20161213b in P-1 #2
REM SHELXT solution in P-1
REM R1 0.181, Rweak 0.022, Alpha 0.074, Orientation as input
REM Formula found by SHELXT: C22 F4 Br2
CELL 0.71073 6.8502 8.065 17.0969 97.18 100.583 100.33
ZERR 2 0.0007 0.0007 0.0016 0.008 0.008 0.008
LATT 1
SFAC C H Br F
UNIT 44 20 4 8
L.S. 10
PLAN 5
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
SHEL 999 0.83
REM
REM
REM
WGHT 0.040600 0.205600
FVAR 0.39996
BR7 3 0.381917 0.981830 0.897486 11.00000 0.03235 0.05107 =
0.02255 -0.00517 0.00471 0.01674
BR8 3 0.284714 0.936376 0.559505 11.00000 0.05128 0.06192 =
0.02962 0.02401 0.01181 0.01800
F12 4 0.373797 1.096983 0.735317 11.00000 0.03960 0.01757 =
0.04273 0.00728 0.01054 0.00686
F11 4 0.184113 0.558023 0.570557 11.00000 0.03862 0.04748 =
0.02756 -0.01516 0.00794 0.00680
F9 4 0.258562 0.595050 0.848891 11.00000 0.04239 0.04538 =
0.03806 0.02370 0.01924 0.01565
F10 4 0.177141 0.406097 0.701206 11.00000 0.04279 0.01651 =
0.06822 0.00205 0.02333 0.00535
C2 1 0.325665 0.926489 0.727184 11.00000 0.01818 0.02193 =
0.02647 0.00429 0.00369 0.00771
C1 1 0.319221 0.848117 0.793980 11.00000 0.01933 0.02616 =
0.01367 -0.01080 -0.00196 0.00483
C16 1 0.225641 0.257462 0.261477 11.00000 0.02097 0.02947 =
0.02530 0.00815 0.00814 0.01478
C26 1 0.126106 -0.018831 0.179932 11.00000 0.02489 0.02084 =
0.03183 0.00517 0.00905 0.01004
AFIX 43
H26 2 0.093860 -0.090385 0.130299 11.00000 -1.20000
AFIX 0
C4 1 0.231677 0.656302 0.643325 11.00000 0.02283 0.03051 =
0.02190 -0.00792 0.00750 0.00571
C23 1 0.182024 0.155250 0.184888 11.00000 0.02672 0.02595 =
0.02593 0.00691 0.01005 0.01446
C15 1 0.216697 0.194504 0.333279 11.00000 0.01827 0.02581 =
0.02902 0.00653 0.00709 0.00916
C19 1 0.306895 0.576690 0.128445 11.00000 0.02333 0.01907 =
0.02838 0.00041 0.00575 0.00567
AFIX 43
H19 2 0.348467 0.688072 0.156164 11.00000 -1.20000
AFIX 0
C13 1 0.207839 0.273988 0.127003 11.00000 0.01942 0.02675 =
0.02394 0.00625 0.00780 0.01411
C27 1 0.118653 -0.087092 0.252378 11.00000 0.02296 0.02635 =
0.04258 0.01160 0.00895 0.01057
AFIX 43
H27 2 0.083438 -0.204889 0.249489 11.00000 -1.20000
AFIX 0
C17 1 0.278762 0.432852 0.255803 11.00000 0.02194 0.02900 =
0.02541 0.00755 0.01083 0.01506
C18 1 0.269324 0.442248 0.169634 11.00000 0.02243 0.02102 =
0.02151 -0.00002 0.00630 0.01182
C6 1 0.268448 0.673317 0.784633 11.00000 0.02015 0.02777 =
0.02211 0.00609 0.00806 0.00940
C22 1 0.184738 0.243441 0.043471 11.00000 0.02210 0.01470 =
0.02787 0.00001 0.00620 0.00467
AFIX 43
H22 2 0.144371 0.132471 0.015216 11.00000 -1.20000
AFIX 0
C20 1 0.282166 0.544486 0.045179 11.00000 0.03668 0.02936 =
0.03368 0.01446 0.01373 0.01313
AFIX 43
H20 2 0.306229 0.635382 0.017287 11.00000 -1.20000
AFIX 0
C28 1 0.161465 0.014561 0.325955 11.00000 0.03467 0.02530 =
0.02444 0.00904 0.00929 0.00503
AFIX 43
H28 2 0.154283 -0.034971 0.371910 11.00000 -1.20000
AFIX 0
C14 1 0.267794 0.319214 0.403818 11.00000 0.02260 0.04862 =
0.02370 0.01056 0.00971 0.00931
AFIX 43
H14 2 0.262992 0.285224 0.453564 11.00000 -1.20000
AFIX 0
C24 1 0.331021 0.549548 0.325877 11.00000 0.02480 0.03241 =
0.03300 0.00514 0.01019 0.01463
AFIX 43
H24 2 0.370016 0.665621 0.324732 11.00000 -1.20000
AFIX 0
C25 1 0.324223 0.489265 0.399876 11.00000 0.02592 0.03852 =
0.02384 -0.00660 0.00210 0.00712
AFIX 43
H25 2 0.359269 0.567818 0.447425 11.00000 -1.20000
AFIX 0
C21 1 0.222539 0.380084 0.003043 11.00000 0.03486 0.02766 =
0.01990 0.00409 0.00729 0.00391
AFIX 43
H21 2 0.207711 0.361062 -0.052715 11.00000 -1.20000
AFIX 0
C3 1 0.280869 0.831321 0.650607 11.00000 0.02617 0.03163 =
0.02352 0.01220 0.00764 0.01432
C5 1 0.224100 0.576936 0.709767 11.00000 0.02171 0.02203 =
0.04107 0.00092 0.00883 0.00633
HKLF 4
REM 20161213b_a.res in P-1
REM R1 = 0.0542 for 2448 Fo > 4sig(Fo) and 0.0808 for all 3299 data
REM 253 parameters refined using 0 restraints
END
WGHT 0.0406 0.2057
REM Highest difference peak 0.491, deepest hole -0.670, 1-sigma level 0.123
Q1 1 0.3348 0.9305 0.5578 11.00000 0.05 0.49
Q2 1 0.2741 1.0435 0.5815 11.00000 0.05 0.49
Q3 1 0.1746 0.8730 0.4997 11.00000 0.05 0.46
Q4 1 0.0711 0.7972 0.8193 11.00000 0.05 0.45
Q5 1 -0.0040 0.2551 0.1538 11.00000 0.05 0.44
REM The information below was added by Olex2.
REM
REM R1 = 0.0542 for 2448 Fo > 4sig(Fo) and 0.0808 for all 8126 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.49, deepest hole -0.67
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0808
REM R1_gt = 0.0542
REM wR_ref = 0.1237
REM GOOF = 1.065
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 8126
REM Reflections_gt = 2448
REM Parameters = n/a
REM Hole = -0.67
REM Peak = 0.49
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.171
_oxdiff_exptl_absorpt_empirical_full_min 0.658
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_20161213a
_database_code_depnum_ccdc_archive 'CCDC 1547634'
_audit_update_record
;
2017-07-20 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_audit_creation_date 2016-12-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common ?
_chemical_name_systematic 1BrPB-FA
_chemical_formula_moiety 'Br C6 F5, C16 H10'
_chemical_formula_sum 'C22 H10 Br F5'
_chemical_formula_weight 449.21
_chemical_absolute_configuration ad
_chemical_melting_point ?
_chemical_oxdiff_formula c1h1f1Br1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 '-x, y+1/2, -z+1/2'
4 'x+1/2, -y+1/2, -z'
_cell_length_a 7.5813(6)
_cell_length_b 7.9328(5)
_cell_length_c 28.450(3)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 1711.0(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 1324
_cell_measurement_temperature 100.01(10)
_cell_measurement_theta_max 25.4370
_cell_measurement_theta_min 3.9350
_exptl_absorpt_coefficient_mu 2.459
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.68799
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.744
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 888
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.2
_exptl_special_details
;
?
;
_diffrn_reflns_av_R_equivalents 0.0523
_diffrn_reflns_av_unetI/netI 0.0825
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 34
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 5387
_diffrn_reflns_theta_full 25.34
_diffrn_reflns_theta_max 25.34
_diffrn_reflns_theta_min 3.44
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 0.9937
_diffrn_measured_fraction_theta_max 0.7351
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -14.00 78.00 1.00 5.00 -- 12.61 19.00 90.00 92
2 \w -10.00 39.00 1.00 5.00 -- 12.61 -99.00-120.00 49
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0658050000
_diffrn_orient_matrix_UB_12 -0.0629663000
_diffrn_orient_matrix_UB_13 -0.0022521000
_diffrn_orient_matrix_UB_21 0.0347189000
_diffrn_orient_matrix_UB_22 -0.0230625000
_diffrn_orient_matrix_UB_23 -0.0222512000
_diffrn_orient_matrix_UB_31 0.0567409000
_diffrn_orient_matrix_UB_32 -0.0591333000
_diffrn_orient_matrix_UB_33 0.0110241000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_reflns_number_gt 2378
_reflns_number_total 2877
_reflns_odcompleteness_completeness 99.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_threshold_expression >2sigma(I)
_computing_cell_refinement 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max 0.362
_refine_diff_density_min -0.447
_refine_diff_density_rms 0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.017(16)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.027
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 253
_refine_ls_number_reflns 2877
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0656
_refine_ls_R_factor_gt 0.0499
_refine_ls_restrained_S_all 1.027
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0979
_refine_ls_wR_factor_ref 0.1063
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C18(H18), C21(H21), C17(H17), C16(H16), C8(H8), C22(H22), C12(H12), C11(H11),
C7(H7), C13(H13)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Br1 Br 0.49420(8) 0.29076(7) 0.68589(2) 0.03714(19) Uani 1 d . . .
F5 F 0.3367(4) -0.0427(4) 0.71806(10) 0.0355(9) Uani 1 d . . .
F3 F 0.4442(4) -0.3624(4) 0.58192(11) 0.0316(8) Uani 1 d . . .
F1 F 0.6355(4) 0.1995(4) 0.58919(11) 0.0343(8) Uani 1 d . . .
F4 F 0.3123(4) -0.3364(4) 0.67049(12) 0.0430(9) Uani 1 d . . .
F2 F 0.6065(4) -0.0939(5) 0.54199(10) 0.0363(9) Uani 1 d . . .
C2 C 0.5543(6) 0.0692(7) 0.60952(18) 0.0213(13) Uani 1 d . . .
C1 C 0.4852(8) 0.0851(6) 0.65430(17) 0.0222(11) Uani 1 d . . .
C19 C 0.5124(8) 0.4091(6) 0.35866(15) 0.0187(11) Uani 1 d . . .
C6 C 0.4042(7) -0.0528(7) 0.67438(17) 0.0233(13) Uani 1 d . . .
C20 C 0.5950(6) 0.3690(7) 0.40521(17) 0.0179(12) Uani 1 d . . .
C18 C 0.4837(6) 0.3221(6) 0.31804(16) 0.0236(11) Uani 1 d . . .
H18 H 0.5168 0.2097 0.3151 0.028 Uiso 1 calc . . R
C5 C 0.3917(6) -0.2026(8) 0.65087(19) 0.0249(12) Uani 1 d . . .
C10 C 0.4994(8) 0.6498(6) 0.40643(16) 0.0206(10) Uani 1 d . . .
C15 C 0.4593(6) 0.5786(6) 0.36193(17) 0.0197(12) Uani 1 d . . .
C4 C 0.4596(6) -0.2156(7) 0.60572(19) 0.0265(13) Uani 1 d . . .
C3 C 0.5396(6) -0.0797(7) 0.58589(18) 0.0246(13) Uani 1 d . . .
C21 C 0.6780(6) 0.2238(7) 0.42079(18) 0.0234(12) Uani 1 d . . .
H21 H 0.6835 0.1284 0.4019 0.028 Uiso 1 calc . . R
C9 C 0.5874(7) 0.5159(7) 0.43342(18) 0.0190(12) Uani 1 d . . .
C17 C 0.4009(7) 0.4096(8) 0.2801(2) 0.0296(14) Uani 1 d . . .
H17 H 0.3807 0.3527 0.2520 0.036 Uiso 1 calc . . R
C16 C 0.3506(7) 0.5745(8) 0.28376(19) 0.0290(14) Uani 1 d . . .
H16 H 0.2971 0.6270 0.2582 0.035 Uiso 1 calc . . R
C14 C 0.3782(6) 0.6666(7) 0.32551(18) 0.0241(13) Uani 1 d . . .
C8 C 0.6621(7) 0.5141(8) 0.47795(19) 0.0263(13) Uani 1 d . . .
H8 H 0.6575 0.6087 0.4972 0.032 Uiso 1 calc . . R
C22 C 0.7532(7) 0.2241(8) 0.46553(19) 0.0290(14) Uani 1 d . . .
H22 H 0.8093 0.1280 0.4768 0.035 Uiso 1 calc . . R
C12 C 0.3711(7) 0.9059(7) 0.3781(2) 0.0294(14) Uani 1 d . . .
H12 H 0.3409 1.0177 0.3836 0.035 Uiso 1 calc . . R
C11 C 0.4553(6) 0.8139(7) 0.4143(2) 0.0269(13) Uani 1 d . . .
H11 H 0.4802 0.8646 0.4430 0.032 Uiso 1 calc . . R
C7 C 0.7443(7) 0.3662(8) 0.49301(18) 0.0295(14) Uani 1 d . . .
H7 H 0.7949 0.3638 0.5228 0.035 Uiso 1 calc . . R
C13 C 0.3327(7) 0.8375(8) 0.3356(2) 0.0331(15) Uani 1 d . . .
H13 H 0.2762 0.9023 0.3129 0.040 Uiso 1 calc . . R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0341(3) 0.0322(3) 0.0451(4) -0.0147(3) -0.0005(4) 0.0015(3)
F5 0.041(2) 0.046(2) 0.0201(17) 0.0085(17) 0.0073(15) 0.0124(18)
F3 0.0334(19) 0.0200(16) 0.0414(18) -0.0140(15) 0.0004(14) -0.0004(14)
F1 0.0303(17) 0.0335(19) 0.0389(18) 0.0087(18) 0.0044(15) -0.0067(17)
F4 0.045(2) 0.027(2) 0.057(2) 0.0165(18) 0.0120(18) -0.0042(17)
F2 0.0339(18) 0.055(2) 0.0205(16) 0.0017(17) 0.0036(15) 0.0067(18)
C2 0.016(3) 0.024(3) 0.024(3) 0.007(2) 0.000(2) 0.005(2)
C1 0.023(3) 0.021(2) 0.023(3) 0.001(2) -0.003(3) 0.002(3)
C19 0.018(2) 0.022(2) 0.016(2) 0.002(2) 0.000(3) -0.001(3)
C6 0.022(3) 0.034(3) 0.014(3) 0.006(3) 0.000(2) 0.010(3)
C20 0.011(2) 0.021(3) 0.022(3) -0.003(3) 0.004(2) -0.006(2)
C18 0.020(3) 0.024(3) 0.028(3) -0.005(2) 0.003(3) -0.003(3)
C5 0.020(3) 0.025(3) 0.030(3) 0.010(3) -0.001(2) 0.003(3)
C10 0.015(2) 0.020(2) 0.026(3) -0.002(2) 0.003(3) -0.003(3)
C15 0.014(3) 0.023(3) 0.022(3) 0.003(2) 0.009(2) -0.002(2)
C4 0.019(3) 0.027(3) 0.034(3) -0.002(3) -0.002(2) 0.002(3)
C3 0.016(3) 0.038(3) 0.021(3) 0.003(3) 0.004(2) 0.006(3)
C21 0.021(3) 0.020(3) 0.029(3) 0.002(3) 0.007(2) -0.003(3)
C9 0.018(3) 0.021(3) 0.018(3) 0.000(2) 0.007(2) -0.002(2)
C17 0.024(3) 0.043(4) 0.022(3) -0.003(3) 0.005(3) -0.014(3)
C16 0.022(3) 0.048(4) 0.017(3) 0.011(3) -0.003(2) -0.005(3)
C14 0.015(3) 0.033(3) 0.025(3) 0.011(3) 0.003(2) -0.003(3)
C8 0.024(3) 0.029(3) 0.026(3) 0.001(3) 0.003(3) -0.005(3)
C22 0.028(3) 0.025(3) 0.034(3) 0.015(3) -0.005(3) -0.008(3)
C12 0.022(3) 0.020(3) 0.047(4) -0.002(3) 0.011(3) 0.000(3)
C11 0.025(3) 0.023(3) 0.033(3) -0.001(3) 0.009(2) 0.000(3)
C7 0.029(3) 0.043(4) 0.016(3) 0.007(3) -0.001(2) -0.014(3)
C13 0.019(3) 0.037(4) 0.043(4) 0.016(3) 0.002(3) -0.001(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
Br1 C1 1.864(5) . ?
F5 C6 1.346(6) . ?
F3 C4 1.352(6) . ?
F1 C2 1.335(6) . ?
F4 C5 1.341(6) . ?
F2 C3 1.353(6) . ?
C2 C1 1.384(7) . ?
C2 C3 1.364(7) . ?
C1 C6 1.379(7) . ?
C19 C20 1.499(7) . ?
C19 C18 1.363(6) . ?
C19 C15 1.407(7) . ?
C6 C5 1.367(8) . ?
C20 C21 1.385(7) . ?
C20 C9 1.416(7) . ?
C18 H18 0.9300 . ?
C18 C17 1.429(7) . ?
C5 C4 1.388(7) . ?
C10 C15 1.420(7) . ?
C10 C9 1.471(7) . ?
C10 C11 1.362(7) . ?
C15 C14 1.393(7) . ?
C4 C3 1.359(7) . ?
C21 H21 0.9300 . ?
C21 C22 1.394(7) . ?
C9 C8 1.388(7) . ?
C17 H17 0.9300 . ?
C17 C16 1.366(8) . ?
C16 H16 0.9300 . ?
C16 C14 1.410(8) . ?
C14 C13 1.428(8) . ?
C8 H8 0.9300 . ?
C8 C7 1.396(8) . ?
C22 H22 0.9300 . ?
C22 C7 1.374(8) . ?
C12 H12 0.9300 . ?
C12 C11 1.414(8) . ?
C12 C13 1.356(8) . ?
C11 H11 0.9300 . ?
C7 H7 0.9300 . ?
C13 H13 0.9300 . ?
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
F1 C2 C1 120.2(5) . . ?
F1 C2 C3 119.7(5) . . ?
C3 C2 C1 120.1(5) . . ?
C2 C1 Br1 120.7(4) . . ?
C6 C1 Br1 120.8(4) . . ?
C6 C1 C2 118.6(5) . . ?
C18 C19 C20 135.1(5) . . ?
C18 C19 C15 119.6(5) . . ?
C15 C19 C20 105.3(4) . . ?
F5 C6 C1 120.3(5) . . ?
F5 C6 C5 118.5(5) . . ?
C5 C6 C1 121.2(5) . . ?
C21 C20 C19 130.5(5) . . ?
C21 C20 C9 121.4(5) . . ?
C9 C20 C19 108.0(4) . . ?
C19 C18 H18 121.1 . . ?
C19 C18 C17 117.7(5) . . ?
C17 C18 H18 121.1 . . ?
F4 C5 C6 121.0(5) . . ?
F4 C5 C4 119.5(5) . . ?
C6 C5 C4 119.5(5) . . ?
C15 C10 C9 106.0(4) . . ?
C11 C10 C15 118.3(5) . . ?
C11 C10 C9 135.7(5) . . ?
C19 C15 C10 112.2(4) . . ?
C14 C15 C19 123.8(5) . . ?
C14 C15 C10 124.0(5) . . ?
F3 C4 C5 119.7(5) . . ?
F3 C4 C3 120.9(5) . . ?
C3 C4 C5 119.4(5) . . ?
F2 C3 C2 119.8(5) . . ?
F2 C3 C4 119.0(5) . . ?
C4 C3 C2 121.2(5) . . ?
C20 C21 H21 120.8 . . ?
C20 C21 C22 118.4(5) . . ?
C22 C21 H21 120.8 . . ?
C20 C9 C10 108.5(4) . . ?
C8 C9 C20 119.5(5) . . ?
C8 C9 C10 132.0(5) . . ?
C18 C17 H17 119.0 . . ?
C16 C17 C18 122.0(5) . . ?
C16 C17 H17 119.0 . . ?
C17 C16 H16 119.4 . . ?
C17 C16 C14 121.3(5) . . ?
C14 C16 H16 119.4 . . ?
C15 C14 C16 115.6(5) . . ?
C15 C14 C13 115.7(5) . . ?
C16 C14 C13 128.7(5) . . ?
C9 C8 H8 120.9 . . ?
C9 C8 C7 118.1(5) . . ?
C7 C8 H8 120.9 . . ?
C21 C22 H22 120.0 . . ?
C7 C22 C21 120.1(5) . . ?
C7 C22 H22 120.0 . . ?
C11 C12 H12 118.7 . . ?
C13 C12 H12 118.7 . . ?
C13 C12 C11 122.6(5) . . ?
C10 C11 C12 119.0(5) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
C8 C7 H7 118.8 . . ?
C22 C7 C8 122.5(5) . . ?
C22 C7 H7 118.8 . . ?
C14 C13 H13 119.8 . . ?
C12 C13 C14 120.5(6) . . ?
C12 C13 H13 119.8 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C1 C6 F5 -2.8(7) . . . . ?
Br1 C1 C6 C5 177.8(4) . . . . ?
F5 C6 C5 F4 0.8(7) . . . . ?
F5 C6 C5 C4 179.7(4) . . . . ?
F3 C4 C3 F2 -1.0(7) . . . . ?
F3 C4 C3 C2 179.4(4) . . . . ?
F1 C2 C1 Br1 3.0(7) . . . . ?
F1 C2 C1 C6 -179.2(5) . . . . ?
F1 C2 C3 F2 -0.4(7) . . . . ?
F1 C2 C3 C4 179.2(4) . . . . ?
F4 C5 C4 F3 0.4(7) . . . . ?
F4 C5 C4 C3 179.8(5) . . . . ?
C2 C1 C6 F5 179.4(4) . . . . ?
C2 C1 C6 C5 0.0(8) . . . . ?
C1 C2 C3 F2 179.5(4) . . . . ?
C1 C2 C3 C4 -0.9(8) . . . . ?
C1 C6 C5 F4 -179.8(5) . . . . ?
C1 C6 C5 C4 -0.9(8) . . . . ?
C19 C20 C21 C22 176.3(5) . . . . ?
C19 C20 C9 C10 0.7(6) . . . . ?
C19 C20 C9 C8 -177.4(4) . . . . ?
C19 C18 C17 C16 -0.3(8) . . . . ?
C19 C15 C14 C16 0.1(8) . . . . ?
C19 C15 C14 C13 179.5(5) . . . . ?
C6 C5 C4 F3 -178.6(4) . . . . ?
C6 C5 C4 C3 0.9(7) . . . . ?
C20 C19 C18 C17 -178.7(5) . . . . ?
C20 C19 C15 C10 -0.4(6) . . . . ?
C20 C19 C15 C14 179.0(4) . . . . ?
C20 C21 C22 C7 -0.2(7) . . . . ?
C20 C9 C8 C7 0.7(7) . . . . ?
C18 C19 C20 C21 3.1(10) . . . . ?
C18 C19 C20 C9 179.1(6) . . . . ?
C18 C19 C15 C10 -179.9(4) . . . . ?
C18 C19 C15 C14 -0.4(8) . . . . ?
C18 C17 C16 C14 0.0(8) . . . . ?
C5 C4 C3 F2 179.6(4) . . . . ?
C5 C4 C3 C2 0.0(8) . . . . ?
C10 C15 C14 C16 179.5(5) . . . . ?
C10 C15 C14 C13 -1.1(7) . . . . ?
C10 C9 C8 C7 -177.0(5) . . . . ?
C15 C19 C20 C21 -176.2(5) . . . . ?
C15 C19 C20 C9 -0.2(6) . . . . ?
C15 C19 C18 C17 0.5(7) . . . . ?
C15 C10 C9 C20 -1.0(6) . . . . ?
C15 C10 C9 C8 176.9(5) . . . . ?
C15 C10 C11 C12 0.3(8) . . . . ?
C15 C14 C13 C12 1.2(7) . . . . ?
C3 C2 C1 Br1 -176.9(4) . . . . ?
C3 C2 C1 C6 0.9(7) . . . . ?
C21 C20 C9 C10 177.2(4) . . . . ?
C21 C20 C9 C8 -1.0(7) . . . . ?
C21 C22 C7 C8 -0.1(8) . . . . ?
C9 C20 C21 C22 0.7(7) . . . . ?
C9 C10 C15 C19 0.9(6) . . . . ?
C9 C10 C15 C14 -178.5(5) . . . . ?
C9 C10 C11 C12 178.9(6) . . . . ?
C9 C8 C7 C22 -0.1(8) . . . . ?
C17 C16 C14 C15 0.1(7) . . . . ?
C17 C16 C14 C13 -179.2(5) . . . . ?
C16 C14 C13 C12 -179.5(5) . . . . ?
C11 C10 C15 C19 179.8(5) . . . . ?
C11 C10 C15 C14 0.4(8) . . . . ?
C11 C10 C9 C20 -179.6(6) . . . . ?
C11 C10 C9 C8 -1.8(11) . . . . ?
C11 C12 C13 C14 -0.5(8) . . . . ?
C13 C12 C11 C10 -0.2(8) . . . . ?
_iucr_refine_instructions_details
;
TITL 20161213a_a.res in P2(1)2(1)2(1)
REM Old TITL 20161213a in P212121 #19
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.117, Rweak 0.102, Alpha 0.008, Orientation as input
REM Flack x = -0.013 ( 0.016 ) from Parsons' quotients
REM Formula found by SHELXT: C8 F5 Br
CELL 0.71073 7.5813 7.9328 28.4496 90 90 90
ZERR 4 0.0006 0.0005 0.0028 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Br F
UNIT 88 40 4 20
L.S. 10
PLAN 5
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
SHEL 999 0.83
REM
REM
REM
WGHT 0.038800
FVAR 0.45280
BR1 3 0.494201 0.290760 0.685886 11.00000 0.03414 0.03217 =
0.04512 -0.01468 -0.00050 0.00152
F5 4 0.336732 -0.042675 0.718064 11.00000 0.04071 0.04581 =
0.02009 0.00853 0.00731 0.01243
F3 4 0.444185 -0.362381 0.581917 11.00000 0.03337 0.01996 =
0.04139 -0.01398 0.00042 -0.00036
F1 4 0.635538 0.199506 0.589186 11.00000 0.03032 0.03354 =
0.03891 0.00872 0.00436 -0.00666
F4 4 0.312270 -0.336353 0.670486 11.00000 0.04481 0.02716 =
0.05700 0.01650 0.01197 -0.00423
F2 4 0.606504 -0.093882 0.541990 11.00000 0.03392 0.05461 =
0.02047 0.00173 0.00363 0.00670
C2 1 0.554328 0.069224 0.609518 11.00000 0.01624 0.02358 =
0.02416 0.00721 -0.00015 0.00471
C1 1 0.485184 0.085115 0.654305 11.00000 0.02292 0.02053 =
0.02304 0.00067 -0.00282 0.00199
C19 1 0.512375 0.409069 0.358657 11.00000 0.01776 0.02212 =
0.01631 0.00170 0.00019 -0.00088
C6 1 0.404206 -0.052816 0.674381 11.00000 0.02245 0.03380 =
0.01366 0.00570 -0.00027 0.01039
C20 1 0.595038 0.368962 0.405206 11.00000 0.01086 0.02084 =
0.02205 -0.00264 0.00358 -0.00610
C18 1 0.483670 0.322147 0.318045 11.00000 0.01985 0.02359 =
0.02750 -0.00511 0.00343 -0.00317
AFIX 43
H18 2 0.516799 0.209749 0.315142 11.00000 -1.20000
AFIX 0
C5 1 0.391682 -0.202614 0.650870 11.00000 0.01983 0.02514 =
0.02971 0.01019 -0.00132 0.00313
C10 1 0.499404 0.649805 0.406430 11.00000 0.01516 0.02006 =
0.02648 -0.00188 0.00300 -0.00274
C15 1 0.459253 0.578567 0.361926 11.00000 0.01446 0.02270 =
0.02183 0.00300 0.00884 -0.00232
C4 1 0.459607 -0.215609 0.605722 11.00000 0.01914 0.02667 =
0.03380 -0.00207 -0.00158 0.00166
C3 1 0.539619 -0.079741 0.585887 11.00000 0.01564 0.03758 =
0.02050 0.00307 0.00362 0.00585
C21 1 0.678030 0.223794 0.420793 11.00000 0.02050 0.02033 =
0.02931 0.00182 0.00670 -0.00259
AFIX 43
H21 2 0.683516 0.128359 0.401863 11.00000 -1.20000
AFIX 0
C9 1 0.587364 0.515872 0.433417 11.00000 0.01829 0.02118 =
0.01751 -0.00035 0.00668 -0.00187
C17 1 0.400931 0.409640 0.280082 11.00000 0.02374 0.04309 =
0.02210 -0.00265 0.00471 -0.01390
AFIX 43
H17 2 0.380741 0.352659 0.252024 11.00000 -1.20000
AFIX 0
C16 1 0.350583 0.574492 0.283758 11.00000 0.02214 0.04831 =
0.01656 0.01118 -0.00297 -0.00467
AFIX 43
H16 2 0.297073 0.626951 0.258238 11.00000 -1.20000
AFIX 0
C14 1 0.378195 0.666624 0.325507 11.00000 0.01479 0.03256 =
0.02488 0.01137 0.00322 -0.00253
C8 1 0.662060 0.514086 0.477946 11.00000 0.02408 0.02864 =
0.02620 0.00056 0.00261 -0.00545
AFIX 43
H8 2 0.657472 0.608721 0.497201 11.00000 -1.20000
AFIX 0
C22 1 0.753158 0.224098 0.465531 11.00000 0.02768 0.02537 =
0.03406 0.01496 -0.00483 -0.00825
AFIX 43
H22 2 0.809332 0.127993 0.476774 11.00000 -1.20000
AFIX 0
C12 1 0.371099 0.905864 0.378067 11.00000 0.02154 0.02020 =
0.04659 -0.00249 0.01055 -0.00044
AFIX 43
H12 2 0.340868 1.017725 0.383618 11.00000 -1.20000
AFIX 0
C11 1 0.455329 0.813877 0.414256 11.00000 0.02469 0.02335 =
0.03260 -0.00130 0.00918 0.00018
AFIX 43
H11 2 0.480245 0.864648 0.442964 11.00000 -1.20000
AFIX 0
C7 1 0.744270 0.366217 0.493010 11.00000 0.02919 0.04303 =
0.01615 0.00740 -0.00139 -0.01389
AFIX 43
H7 2 0.794938 0.363824 0.522773 11.00000 -1.20000
AFIX 0
C13 1 0.332651 0.837499 0.335598 11.00000 0.01945 0.03731 =
0.04259 0.01632 0.00218 -0.00148
AFIX 43
H13 2 0.276237 0.902342 0.312889 11.00000 -1.20000
HKLF 4
REM 20161213a_a.res in P2(1)2(1)2(1)
REM R1 = 0.0499 for 2378 Fo > 4sig(Fo) and 0.0656 for all 2877 data
REM 253 parameters refined using 0 restraints
END
WGHT 0.0388 0.0000
REM Highest difference peak 0.362, deepest hole -0.447, 1-sigma level 0.082
Q1 1 0.6379 -0.3688 0.5892 11.00000 0.05 0.36
Q2 1 0.3850 -0.3592 0.5958 11.00000 0.05 0.31
Q3 1 0.4640 0.2813 0.5974 11.00000 0.05 0.31
Q4 1 0.4693 0.0699 0.6352 11.00000 0.05 0.30
Q5 1 0.4157 -0.2872 0.7216 11.00000 0.05 0.29
REM The information below was added by Olex2.
REM
REM R1 = 0.0499 for 2378 Fo > 4sig(Fo) and 0.0656 for all 6334 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.36, deepest hole -0.45
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0656
REM R1_gt = 0.0499
REM wR_ref = 0.1063
REM GOOF = 1.027
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 6334
REM Reflections_gt = 2378
REM Parameters = n/a
REM Hole = -0.45
REM Peak = 0.36
REM Flack = -0.017(16)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.307
_oxdiff_exptl_absorpt_empirical_full_min 0.750
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_20161209a
_database_code_depnum_ccdc_archive 'CCDC 1547626'
_audit_update_record
;
2017-07-20 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_audit_creation_date 2016-12-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common ?
_chemical_name_systematic 1ClPB-FA
_chemical_formula_moiety 'C6 Cl F5, C16 H10'
_chemical_formula_sum 'C22 H10 Cl F5'
_chemical_formula_weight 404.75
_chemical_absolute_configuration ad
_chemical_melting_point ?
_chemical_oxdiff_formula c1h1f1Cl1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 '-x, y+1/2, -z+1/2'
4 'x+1/2, -y+1/2, -z'
_cell_length_a 7.5282(2)
_cell_length_b 7.8131(2)
_cell_length_c 28.2918(9)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 1664.08(8)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 11252
_cell_measurement_temperature 100.01(10)
_cell_measurement_theta_max 29.9900
_cell_measurement_theta_min 3.7030
_exptl_absorpt_coefficient_mu 0.287
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.42422
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.616
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 816
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.35
_exptl_special_details
;
?
;
_diffrn_reflns_av_R_equivalents 0.0386
_diffrn_reflns_av_unetI/netI 0.0200
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 34
_diffrn_reflns_limit_l_min -34
_diffrn_reflns_number 24501
_diffrn_reflns_theta_full 25.34
_diffrn_reflns_theta_max 25.34
_diffrn_reflns_theta_min 3.39
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 0.9951
_diffrn_measured_fraction_theta_max 0.8859
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w 4.00 45.00 1.00 3.00 -- 12.76 -77.00 90.00 41
2 \w -14.00 81.00 1.00 3.00 -- 12.76 77.00-180.00 95
3 \w 3.00 53.00 1.00 3.00 -- 12.45 -99.00 -60.00 50
4 \w 9.00 39.00 1.00 3.00 -- 12.45 -99.00 60.00 30
5 \w 9.00 37.00 1.00 3.00 -- 12.45 -37.00 30.00 28
6 \w -36.00 5.00 1.00 3.00 -- 12.45 -37.00 30.00 41
7 \w -23.00 85.00 1.00 3.00 -- 12.45 19.00 150.00 108
8 \w -19.00 89.00 1.00 3.00 -- 12.45 77.00 -30.00 108
9 \w 19.00 47.00 1.00 3.00 -- 14.00 -77.00 28.48 28
10 \w -59.00 -4.00 1.00 3.00 -- 14.00 -77.00 28.48 55
11 \w -34.00 50.00 1.00 3.00 -- 14.00 -87.00-156.41 84
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0307452000
_diffrn_orient_matrix_UB_12 0.0610167000
_diffrn_orient_matrix_UB_13 0.0166514000
_diffrn_orient_matrix_UB_21 0.0232740000
_diffrn_orient_matrix_UB_22 -0.0671530000
_diffrn_orient_matrix_UB_23 0.0157021000
_diffrn_orient_matrix_UB_31 0.0859837000
_diffrn_orient_matrix_UB_32 -0.0036261000
_diffrn_orient_matrix_UB_33 -0.0102112000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_reflns_number_gt 2981
_reflns_number_total 3031
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_threshold_expression >2sigma(I)
_computing_cell_refinement 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max 0.178
_refine_diff_density_min -0.223
_refine_diff_density_rms 0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.02(5)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.110
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 253
_refine_ls_number_reflns 3031
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0260
_refine_ls_R_factor_gt 0.0255
_refine_ls_restrained_S_all 1.110
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.4476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0639
_refine_ls_wR_factor_ref 0.0643
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C8(H8), C9(H9), C17(H17), C12(H12), C22(H22), C7(H7), C19(H19), C14(H14),
C13(H13), C18(H18)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Cl1 Cl 0.50869(6) 0.27772(5) 0.313973(16) 0.02470(12) Uani 1 d . . .
F5 F 0.36801(13) 0.20906(12) 0.40906(4) 0.0229(2) Uani 1 d . . .
F4 F 0.39362(13) -0.08706(14) 0.45793(3) 0.0233(2) Uani 1 d . . .
F3 F 0.55533(14) -0.36298(13) 0.41835(4) 0.0264(3) Uani 1 d . . .
F1 F 0.66417(14) -0.04689(14) 0.28018(3) 0.0248(2) Uani 1 d . . .
F2 F 0.68727(14) -0.34300(13) 0.32917(4) 0.0271(3) Uani 1 d . . .
C4 C 0.5417(2) -0.2164(2) 0.39393(6) 0.0180(4) Uani 1 d . . .
C21 C 0.4138(2) 0.5148(2) 0.56699(6) 0.0139(3) Uani 1 d . . .
C2 C 0.5968(2) -0.0549(2) 0.32409(6) 0.0172(4) Uani 1 d . . .
C8 C 0.2451(2) 0.2202(2) 0.53545(6) 0.0199(4) Uani 1 d . . .
H8 H 0.1881 0.1224 0.5244 0.024 Uiso 1 calc . . R
C10 C 0.4049(2) 0.3668(2) 0.59604(6) 0.0140(3) Uani 1 d . . .
C6 C 0.4473(2) 0.0741(2) 0.38910(6) 0.0154(3) Uani 1 d . . .
C5 C 0.4596(2) -0.0768(2) 0.41404(6) 0.0167(4) Uani 1 d . . .
C3 C 0.6099(2) -0.2059(2) 0.34870(6) 0.0179(3) Uani 1 d . . .
C20 C 0.5035(2) 0.65185(19) 0.59395(6) 0.0146(3) Uani 1 d . . .
C15 C 0.6276(2) 0.6709(2) 0.67513(6) 0.0171(4) Uani 1 d . . .
C9 C 0.3205(2) 0.2204(2) 0.58030(6) 0.0165(3) Uani 1 d . . .
H9 H 0.3143 0.1236 0.5994 0.020 Uiso 1 calc . . R
C16 C 0.5442(2) 0.5814(2) 0.63866(6) 0.0146(3) Uani 1 d . . .
C11 C 0.4890(2) 0.4084(2) 0.64192(6) 0.0144(3) Uani 1 d . . .
C17 C 0.6726(2) 0.8443(2) 0.66506(6) 0.0208(4) Uani 1 d . . .
H17 H 0.7278 0.9107 0.6880 0.025 Uiso 1 calc . . R
C12 C 0.5202(2) 0.3218(2) 0.68327(6) 0.0171(3) Uani 1 d . . .
H12 H 0.4868 0.2078 0.6865 0.020 Uiso 1 calc . . R
C22 C 0.3383(2) 0.5134(2) 0.52214(6) 0.0180(4) Uani 1 d . . .
H22 H 0.3440 0.6095 0.5028 0.022 Uiso 1 calc . . R
C7 C 0.2538(2) 0.3645(2) 0.50695(6) 0.0207(4) Uani 1 d . . .
H7 H 0.2023 0.3618 0.4771 0.025 Uiso 1 calc . . R
C19 C 0.5497(2) 0.8193(2) 0.58512(6) 0.0187(4) Uani 1 d . . .
H19 H 0.5258 0.8695 0.5560 0.022 Uiso 1 calc . . R
C1 C 0.5174(2) 0.0874(2) 0.34394(6) 0.0165(3) Uani 1 d . . .
C14 C 0.6573(2) 0.5776(2) 0.71753(6) 0.0203(4) Uani 1 d . . .
H14 H 0.7127 0.6305 0.7430 0.024 Uiso 1 calc . . R
C13 C 0.6047(2) 0.4099(2) 0.72099(6) 0.0200(4) Uani 1 d . . .
H13 H 0.6251 0.3517 0.7491 0.024 Uiso 1 calc . . R
C18 C 0.6350(2) 0.9135(2) 0.62180(7) 0.0220(4) Uani 1 d . . .
H18 H 0.6664 1.0267 0.6161 0.026 Uiso 1 calc . . R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0249(2) 0.0201(2) 0.0291(2) 0.00931(18) -0.00085(19) -0.00180(19)
F5 0.0215(5) 0.0212(5) 0.0260(5) -0.0066(5) 0.0012(4) 0.0052(4)
F4 0.0232(5) 0.0327(6) 0.0140(5) 0.0015(4) 0.0031(4) -0.0012(5)
F3 0.0296(6) 0.0189(5) 0.0306(6) 0.0098(5) 0.0000(5) 0.0020(4)
F1 0.0272(6) 0.0328(6) 0.0143(5) -0.0041(5) 0.0054(4) -0.0061(5)
F2 0.0292(5) 0.0185(5) 0.0336(6) -0.0088(5) 0.0070(5) 0.0023(5)
C4 0.0153(8) 0.0155(7) 0.0232(9) 0.0044(7) -0.0027(7) -0.0018(7)
C21 0.0116(7) 0.0161(8) 0.0140(8) -0.0001(7) 0.0036(6) 0.0032(7)
C2 0.0144(8) 0.0242(8) 0.0130(8) -0.0033(7) 0.0002(6) -0.0053(7)
C8 0.0176(8) 0.0187(8) 0.0235(9) -0.0098(8) 0.0004(7) 0.0020(7)
C10 0.0121(7) 0.0157(8) 0.0143(8) -0.0005(7) 0.0028(6) 0.0029(6)
C6 0.0121(8) 0.0173(8) 0.0169(8) -0.0050(7) -0.0002(6) -0.0006(7)
C5 0.0119(8) 0.0254(9) 0.0129(8) 0.0002(7) -0.0011(6) -0.0025(7)
C3 0.0140(7) 0.0176(8) 0.0221(9) -0.0067(7) -0.0006(7) -0.0011(7)
C20 0.0113(7) 0.0150(7) 0.0176(8) -0.0002(7) 0.0032(7) 0.0038(7)
C15 0.0120(7) 0.0197(8) 0.0195(8) -0.0041(7) 0.0021(7) 0.0031(7)
C9 0.0158(7) 0.0157(8) 0.0181(8) -0.0016(7) 0.0035(7) 0.0015(7)
C16 0.0106(7) 0.0168(8) 0.0163(8) -0.0022(7) 0.0033(6) 0.0030(7)
C11 0.0116(7) 0.0162(8) 0.0153(8) -0.0008(6) 0.0045(7) 0.0023(7)
C17 0.0145(8) 0.0206(9) 0.0272(9) -0.0097(8) 0.0019(7) -0.0005(8)
C12 0.0169(8) 0.0164(8) 0.0179(8) 0.0018(7) 0.0023(7) 0.0033(7)
C22 0.0184(8) 0.0216(9) 0.0142(8) 0.0021(7) 0.0038(7) 0.0054(7)
C7 0.0196(8) 0.0303(10) 0.0123(8) -0.0057(8) -0.0001(7) 0.0070(8)
C19 0.0171(8) 0.0167(8) 0.0223(9) 0.0032(7) 0.0048(7) 0.0017(7)
C1 0.0147(8) 0.0165(8) 0.0184(8) 0.0028(6) -0.0042(7) -0.0036(7)
C14 0.0147(8) 0.0305(10) 0.0156(8) -0.0060(8) -0.0008(7) 0.0022(8)
C13 0.0186(9) 0.0283(9) 0.0132(8) 0.0031(7) 0.0012(7) 0.0053(8)
C18 0.0184(8) 0.0143(8) 0.0334(10) -0.0011(7) 0.0059(8) -0.0013(7)
_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
Cl1 C1 1.7128(16) . ?
F5 C6 1.3368(19) . ?
F4 C5 1.3397(19) . ?
F3 C4 1.341(2) . ?
F1 C2 1.3433(19) . ?
F2 C3 1.3383(19) . ?
C4 C5 1.377(2) . ?
C4 C3 1.382(2) . ?
C21 C10 1.421(2) . ?
C21 C20 1.478(2) . ?
C21 C22 1.390(2) . ?
C2 C3 1.374(3) . ?
C2 C1 1.381(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.390(2) . ?
C8 C7 1.388(3) . ?
C10 C9 1.382(2) . ?
C10 C11 1.480(2) . ?
C6 C5 1.377(2) . ?
C6 C1 1.387(2) . ?
C20 C16 1.413(2) . ?
C20 C19 1.376(2) . ?
C15 C16 1.396(2) . ?
C15 C17 1.425(2) . ?
C15 C14 1.421(2) . ?
C9 H9 0.9300 . ?
C16 C11 1.417(2) . ?
C11 C12 1.372(2) . ?
C17 H17 0.9300 . ?
C17 C18 1.368(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.420(2) . ?
C22 H22 0.9300 . ?
C22 C7 1.394(3) . ?
C7 H7 0.9300 . ?
C19 H19 0.9300 . ?
C19 C18 1.425(3) . ?
C14 H14 0.9300 . ?
C14 C13 1.373(3) . ?
C13 H13 0.9300 . ?
C18 H18 0.9300 . ?
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
F3 C4 C5 119.87(15) . . ?
F3 C4 C3 119.96(15) . . ?
C5 C4 C3 120.17(16) . . ?
C10 C21 C20 108.24(14) . . ?
C22 C21 C10 120.16(15) . . ?
C22 C21 C20 131.56(15) . . ?
F1 C2 C3 118.77(15) . . ?
F1 C2 C1 120.13(15) . . ?
C3 C2 C1 121.10(15) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.69(17) . . ?
C21 C10 C11 107.95(14) . . ?
C9 C10 C21 120.62(15) . . ?
C9 C10 C11 131.36(15) . . ?
F5 C6 C5 119.28(15) . . ?
F5 C6 C1 120.01(15) . . ?
C5 C6 C1 120.72(15) . . ?
F4 C5 C4 120.12(15) . . ?
F4 C5 C6 120.07(15) . . ?
C4 C5 C6 119.80(15) . . ?
F2 C3 C4 119.77(16) . . ?
F2 C3 C2 120.64(15) . . ?
C2 C3 C4 119.58(16) . . ?
C16 C20 C21 106.19(14) . . ?
C19 C20 C21 135.25(16) . . ?
C19 C20 C16 118.56(16) . . ?
C16 C15 C17 115.82(16) . . ?
C16 C15 C14 115.95(16) . . ?
C14 C15 C17 128.23(17) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 C8 118.83(16) . . ?
C10 C9 H9 120.6 . . ?
C20 C16 C11 111.49(14) . . ?
C15 C16 C20 124.32(16) . . ?
C15 C16 C11 124.19(16) . . ?
C16 C11 C10 106.14(14) . . ?
C12 C11 C10 135.46(15) . . ?
C12 C11 C16 118.40(15) . . ?
C15 C17 H17 119.8 . . ?
C18 C17 C15 120.36(17) . . ?
C18 C17 H17 119.8 . . ?
C11 C12 H12 120.7 . . ?
C11 C12 C13 118.60(15) . . ?
C13 C12 H12 120.7 . . ?
C21 C22 H22 120.8 . . ?
C21 C22 C7 118.31(16) . . ?
C7 C22 H22 120.8 . . ?
C8 C7 C22 121.38(16) . . ?
C8 C7 H7 119.3 . . ?
C22 C7 H7 119.3 . . ?
C20 C19 H19 120.9 . . ?
C20 C19 C18 118.20(16) . . ?
C18 C19 H19 120.9 . . ?
C2 C1 Cl1 120.93(13) . . ?
C2 C1 C6 118.62(15) . . ?
C6 C1 Cl1 120.45(13) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 C15 120.29(16) . . ?
C13 C14 H14 119.9 . . ?
C12 C13 H13 118.7 . . ?
C14 C13 C12 122.58(16) . . ?
C14 C13 H13 118.7 . . ?
C17 C18 C19 122.72(16) . . ?
C17 C18 H18 118.6 . . ?
C19 C18 H18 118.6 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F5 C6 C5 F4 -0.4(2) . . . . ?
F5 C6 C5 C4 -179.70(14) . . . . ?
F5 C6 C1 Cl1 1.8(2) . . . . ?
F5 C6 C1 C2 -179.30(14) . . . . ?
F3 C4 C5 F4 0.1(2) . . . . ?
F3 C4 C5 C6 179.32(14) . . . . ?
F3 C4 C3 F2 0.9(2) . . . . ?
F3 C4 C3 C2 -179.40(15) . . . . ?
F1 C2 C3 F2 -0.5(2) . . . . ?
F1 C2 C3 C4 179.88(14) . . . . ?
F1 C2 C1 Cl1 -1.9(2) . . . . ?
F1 C2 C1 C6 179.20(14) . . . . ?
C21 C10 C9 C8 0.2(2) . . . . ?
C21 C10 C11 C16 0.43(17) . . . . ?
C21 C10 C11 C12 179.89(18) . . . . ?
C21 C20 C16 C15 -178.97(15) . . . . ?
C21 C20 C16 C11 0.79(18) . . . . ?
C21 C20 C19 C18 178.81(17) . . . . ?
C21 C22 C7 C8 -0.2(2) . . . . ?
C10 C21 C20 C16 -0.50(18) . . . . ?
C10 C21 C20 C19 -179.88(17) . . . . ?
C10 C21 C22 C7 0.4(2) . . . . ?
C10 C11 C12 C13 -178.77(17) . . . . ?
C5 C4 C3 F2 -179.07(14) . . . . ?
C5 C4 C3 C2 0.6(2) . . . . ?
C5 C6 C1 Cl1 -177.65(13) . . . . ?
C5 C6 C1 C2 1.3(2) . . . . ?
C3 C4 C5 F4 -179.92(14) . . . . ?
C3 C4 C5 C6 -0.7(2) . . . . ?
C3 C2 C1 Cl1 177.56(13) . . . . ?
C3 C2 C1 C6 -1.4(2) . . . . ?
C20 C21 C10 C9 177.35(14) . . . . ?
C20 C21 C10 C11 0.04(18) . . . . ?
C20 C21 C22 C7 -176.73(16) . . . . ?
C20 C16 C11 C10 -0.77(18) . . . . ?
C20 C16 C11 C12 179.66(15) . . . . ?
C20 C19 C18 C17 0.1(2) . . . . ?
C15 C16 C11 C10 178.99(15) . . . . ?
C15 C16 C11 C12 -0.6(2) . . . . ?
C15 C17 C18 C19 0.4(3) . . . . ?
C15 C14 C13 C12 0.3(3) . . . . ?
C9 C8 C7 C22 0.1(3) . . . . ?
C9 C10 C11 C16 -176.49(16) . . . . ?
C9 C10 C11 C12 3.0(3) . . . . ?
C16 C20 C19 C18 -0.5(2) . . . . ?
C16 C15 C17 C18 -0.4(2) . . . . ?
C16 C15 C14 C13 -0.2(2) . . . . ?
C16 C11 C12 C13 0.6(2) . . . . ?
C11 C10 C9 C8 176.82(16) . . . . ?
C11 C12 C13 C14 -0.5(2) . . . . ?
C17 C15 C16 C20 -0.1(2) . . . . ?
C17 C15 C16 C11 -179.82(15) . . . . ?
C17 C15 C14 C13 180.00(16) . . . . ?
C22 C21 C10 C9 -0.4(2) . . . . ?
C22 C21 C10 C11 -177.67(14) . . . . ?
C22 C21 C20 C16 176.86(17) . . . . ?
C22 C21 C20 C19 -2.5(3) . . . . ?
C7 C8 C9 C10 -0.1(2) . . . . ?
C19 C20 C16 C15 0.5(2) . . . . ?
C19 C20 C16 C11 -179.70(14) . . . . ?
C1 C2 C3 F2 -179.90(14) . . . . ?
C1 C2 C3 C4 0.4(2) . . . . ?
C1 C6 C5 F4 178.97(14) . . . . ?
C1 C6 C5 C4 -0.3(2) . . . . ?
C14 C15 C16 C20 -179.95(15) . . . . ?
C14 C15 C16 C11 0.3(2) . . . . ?
C14 C15 C17 C18 179.48(16) . . . . ?
_iucr_refine_instructions_details
;
TITL 20161209a_a.res in P2(1)2(1)2(1)
REM Old TITL 20161209a in P21212 #18
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.072, Rweak 0.078, Alpha 0.002, Orientation as input
REM Flack x = 0.037 ( 0.020 ) from Parsons' quotients
REM Formula found by SHELXT: C16 F5 Cl
CELL 0.71073 7.5282 7.8131 28.2918 90 90 90
ZERR 4 0.0002 0.0002 0.0009 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Cl F
UNIT 88 40 4 20
L.S. 50
PLAN 5
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
SHEL 999 0.83
REM
REM
REM
WGHT 0.031900 0.447600
FVAR 0.53423
CL1 3 0.508693 0.277723 0.313973 11.00000 0.02494 0.02010 =
0.02906 0.00931 -0.00085 -0.00180
F5 4 0.368014 0.209064 0.409065 11.00000 0.02148 0.02119 =
0.02603 -0.00655 0.00122 0.00516
F4 4 0.393622 -0.087060 0.457927 11.00000 0.02319 0.03275 =
0.01404 0.00151 0.00309 -0.00121
F3 4 0.555333 -0.362982 0.418355 11.00000 0.02961 0.01885 =
0.03064 0.00982 0.00004 0.00204
F1 4 0.664169 -0.046889 0.280181 11.00000 0.02723 0.03284 =
0.01427 -0.00414 0.00541 -0.00610
F2 4 0.687266 -0.342997 0.329174 11.00000 0.02916 0.01846 =
0.03365 -0.00881 0.00696 0.00228
C4 1 0.541650 -0.216436 0.393934 11.00000 0.01529 0.01552 =
0.02321 0.00436 -0.00269 -0.00184
C21 1 0.413808 0.514799 0.566989 11.00000 0.01156 0.01614 =
0.01401 -0.00011 0.00365 0.00323
C2 1 0.596771 -0.054859 0.324090 11.00000 0.01439 0.02420 =
0.01299 -0.00332 0.00024 -0.00531
C8 1 0.245069 0.220239 0.535447 11.00000 0.01762 0.01867 =
0.02352 -0.00982 0.00039 0.00201
AFIX 43
H8 2 0.188125 0.122431 0.524429 11.00000 -1.20000
AFIX 0
C10 1 0.404865 0.366759 0.596039 11.00000 0.01206 0.01566 =
0.01429 -0.00049 0.00282 0.00289
C6 1 0.447276 0.074095 0.389104 11.00000 0.01214 0.01727 =
0.01688 -0.00496 -0.00020 -0.00056
C5 1 0.459574 -0.076811 0.414038 11.00000 0.01187 0.02542 =
0.01294 0.00024 -0.00109 -0.00247
C3 1 0.609899 -0.205929 0.348695 11.00000 0.01404 0.01760 =
0.02209 -0.00671 -0.00065 -0.00115
C20 1 0.503527 0.651850 0.593952 11.00000 0.01134 0.01497 =
0.01757 -0.00017 0.00324 0.00379
C15 1 0.627635 0.670927 0.675128 11.00000 0.01201 0.01970 =
0.01946 -0.00405 0.00206 0.00309
C9 1 0.320524 0.220354 0.580303 11.00000 0.01581 0.01573 =
0.01806 -0.00163 0.00349 0.00152
AFIX 43
H9 2 0.314343 0.123605 0.599381 11.00000 -1.20000
AFIX 0
C16 1 0.544198 0.581389 0.638658 11.00000 0.01062 0.01678 =
0.01626 -0.00221 0.00335 0.00300
C11 1 0.488965 0.408394 0.641921 11.00000 0.01162 0.01619 =
0.01533 -0.00081 0.00449 0.00227
C17 1 0.672604 0.844280 0.665063 11.00000 0.01448 0.02060 =
0.02718 -0.00966 0.00187 -0.00049
AFIX 43
H17 2 0.727841 0.910731 0.688036 11.00000 -1.20000
AFIX 0
C12 1 0.520225 0.321812 0.683271 11.00000 0.01688 0.01640 =
0.01792 0.00184 0.00234 0.00326
AFIX 43
H12 2 0.486831 0.207824 0.686535 11.00000 -1.20000
AFIX 0
C22 1 0.338279 0.513441 0.522139 11.00000 0.01838 0.02160 =
0.01416 0.00207 0.00379 0.00542
AFIX 43
H22 2 0.343964 0.609461 0.502771 11.00000 -1.20000
AFIX 0
C7 1 0.253840 0.364531 0.506946 11.00000 0.01959 0.03025 =
0.01232 -0.00570 -0.00012 0.00699
AFIX 43
H7 2 0.202294 0.361816 0.477082 11.00000 -1.20000
AFIX 0
C19 1 0.549651 0.819265 0.585124 11.00000 0.01713 0.01667 =
0.02228 0.00318 0.00483 0.00165
AFIX 43
H19 2 0.525786 0.869550 0.556014 11.00000 -1.20000
AFIX 0
C1 1 0.517431 0.087424 0.343940 11.00000 0.01471 0.01648 =
0.01837 0.00283 -0.00419 -0.00365
C14 1 0.657324 0.577632 0.717530 11.00000 0.01472 0.03053 =
0.01564 -0.00602 -0.00082 0.00218
AFIX 43
H14 2 0.712677 0.630464 0.743039 11.00000 -1.20000
AFIX 0
C13 1 0.604662 0.409918 0.720992 11.00000 0.01855 0.02831 =
0.01319 0.00307 0.00123 0.00528
AFIX 43
H13 2 0.625074 0.351693 0.749143 11.00000 -1.20000
AFIX 0
C18 1 0.634982 0.913502 0.621799 11.00000 0.01840 0.01429 =
0.03339 -0.00108 0.00591 -0.00131
AFIX 43
H18 2 0.666380 1.026744 0.616077 11.00000 -1.20000
HKLF 4
REM 20161209a_a.res in P2(1)2(1)2(1)
REM R1 = 0.0255 for 2981 Fo > 4sig(Fo) and 0.0260 for all 3031 data
REM 253 parameters refined using 0 restraints
END
WGHT 0.0319 0.4476
REM Highest difference peak 0.178, deepest hole -0.223, 1-sigma level 0.043
Q1 1 0.5309 -0.1424 0.3333 11.00000 0.05 0.18
Q2 1 0.4366 0.0640 0.3576 11.00000 0.05 0.17
Q3 1 0.4075 -0.0281 0.3948 11.00000 0.05 0.16
Q4 1 0.5186 0.4931 0.6425 11.00000 0.05 0.16
Q5 1 0.5357 -0.1386 0.4047 11.00000 0.05 0.16
REM The information below was added by Olex2.
REM
REM R1 = 0.0255 for 2981 Fo > 4sig(Fo) and 0.0260 for all 29095 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.18, deepest hole -0.22
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0260
REM R1_gt = 0.0255
REM wR_ref = 0.0643
REM GOOF = 1.110
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 29095
REM Reflections_gt = 2981
REM Parameters = n/a
REM Hole = -0.22
REM Peak = 0.18
REM Flack = 0.02(5)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.032
_oxdiff_exptl_absorpt_empirical_full_min 0.672