 
data_dgh1910 

# start Validation Reply Form
_vrf_PLAT341_dgh1910
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0235 Ang.  
RESPONSE: The crystal used for data collection was rather weakly diffracting 
at high angles, even with long exposure times for the high angle frame sets.
As a result, the resolution of the data set is reduced, and Rint is higher 
than normal.
;
# end Validation Reply Form 
  
_audit_creation_method            'SHELXL-2017/1' 
_shelx_SHELXL_version_number      '2017/1' 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety           
 'C18 H15 B Br2 F3 K O2' 
_chemical_formula_sum 
 'C18 H15 B Br2 F3 K O2' 
_chemical_formula_weight          530.03 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'B'  'B'   0.0090   0.0039 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'F'  'F'   0.0727   0.0534 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'K'  'K'   0.3868   1.0657 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Br'  'Br'  -0.6763   1.2805 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_space_group_crystal_system       orthorhombic 
_space_group_IT_number            18 
_space_group_name_H-M_alt         'P 21 21 2' 
_space_group_name_Hall            'P 2 2ab' 
  
_shelx_space_group_comment 
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
; 
  
loop_ 
 _space_group_symop_operation_xyz 
 'x, y, z' 
 '-x, -y, z' 
 '-x+1/2, y+1/2, -z' 
 'x+1/2, -y+1/2, -z' 
  
_cell_length_a                    20.0712(12) 
_cell_length_b                    30.159(2) 
_cell_length_c                    6.8657(5) 
_cell_angle_alpha                 90 
_cell_angle_beta                  90 
_cell_angle_gamma                 90 
_cell_volume                      4156.0(5) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     4315 
_cell_measurement_theta_min       2.64 
_cell_measurement_theta_max       64.36 
  
_exptl_crystal_description        needle 
_exptl_crystal_colour             colourless 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     1.694 
_exptl_crystal_F_000              2080 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.420 
_exptl_crystal_size_mid           0.042 
_exptl_crystal_size_min           0.029 
_exptl_absorpt_coefficient_mu     7.078 
_shelx_estimated_absorpt_T_min    0.155 
_shelx_estimated_absorpt_T_max    0.821 
_exptl_absorpt_correction_type    numerical 
_exptl_absorpt_correction_T_min   0.1627 
_exptl_absorpt_correction_T_max   0.6193 
_exptl_absorpt_process_details     
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
; 
_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_source                    ? 
_diffrn_measurement_device_type   'Bruker APEX-II CCD' 
_diffrn_measurement_method        'φ and ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             20900 
_diffrn_reflns_av_unetI/netI      0.1192 
_diffrn_reflns_av_R_equivalents   0.1247 
_diffrn_reflns_limit_h_min        -21 
_diffrn_reflns_limit_h_max        24 
_diffrn_reflns_limit_k_min        -36 
_diffrn_reflns_limit_k_max        33 
_diffrn_reflns_limit_l_min        -8 
_diffrn_reflns_limit_l_max        8 
_diffrn_reflns_theta_min          2.644 
_diffrn_reflns_theta_max          68.252 
_diffrn_reflns_theta_full         67.679 
_diffrn_measured_fraction_theta_max   0.993 
_diffrn_measured_fraction_theta_full  0.993 
_diffrn_reflns_Laue_measured_fraction_max    0.993 
_diffrn_reflns_Laue_measured_fraction_full   0.993 
_diffrn_reflns_point_group_measured_fraction_max   0.996 
_diffrn_reflns_point_group_measured_fraction_full  0.996 
_reflns_number_total              7566 
_reflns_number_gt                 4342 
_reflns_threshold_expression      'I > 2σ(I)' 
_reflns_Friedel_coverage          0.761 
_reflns_Friedel_fraction_max      0.999 
_reflns_Friedel_fraction_full     1.000 
  
_reflns_special_details 
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
; 
  
_computing_data_collection        'Bruker APEX2' 
_computing_cell_refinement        'Bruker SAINT' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'SHELXT-2014/5 (Sheldrick 2015)' 
_computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
_refine_special_details 
; 
 Refined as a 2-component inversion twin. 
; 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.0955P)²] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      dual 
_atom_sites_solution_secondary    ? 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        . 
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
; 
_refine_ls_abs_structure_Flack    0.08(4) 
_chemical_absolute_configuration  ad 
_refine_ls_number_reflns          7566 
_refine_ls_number_parameters      488 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1170 
_refine_ls_R_factor_gt            0.0775 
_refine_ls_wR_factor_ref          0.2111 
_refine_ls_wR_factor_gt           0.1877 
_refine_ls_goodness_of_fit_ref    0.941 
_refine_ls_restrained_S_all       0.941 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_site_symmetry_order 
 _atom_site_calc_flag 
 _atom_site_refinement_flags_posn 
 _atom_site_refinement_flags_adp 
 _atom_site_refinement_flags_occupancy 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Br1A Br 0.87599(14) 0.31309(8) -0.1680(5) 0.1103(9) Uani 1 1 d . . . . . 
Br2A Br 1.02607(10) 0.57625(12) 0.6535(4) 0.1331(13) Uani 1 1 d . . . . . 
F1A F 0.5677(3) 0.5228(3) -0.3479(11) 0.0503(19) Uani 1 1 d . . . . . 
F2A F 0.6365(3) 0.5012(3) -0.1001(10) 0.0492(18) Uani 1 1 d . . . . . 
F3A F 0.5792(3) 0.5664(3) -0.0869(10) 0.053(2) Uani 1 1 d . . . . . 
O1A O 0.7145(4) 0.5662(4) 0.1586(14) 0.055(2) Uani 1 1 d . . . . . 
O2A O 0.7880(4) 0.5267(3) -0.0166(12) 0.046(2) Uani 1 1 d . . . . . 
C1A C 0.6762(6) 0.5631(5) -0.3183(19) 0.044(3) Uani 1 1 d . . . . . 
H1A H 0.695770 0.545235 -0.426805 0.053 Uiso 1 1 calc R U . . . 
C2A C 0.7309(6) 0.5827(5) -0.1801(19) 0.044(3) Uani 1 1 d . . . . . 
H2A H 0.773976 0.584922 -0.252628 0.053 Uiso 1 1 calc R U . . . 
C3A C 0.6938(8) 0.6272(5) -0.195(3) 0.071(5) Uani 1 1 d . . . . . 
H3AA H 0.662615 0.632686 -0.085569 0.086 Uiso 1 1 calc R U . . . 
H3AB H 0.723538 0.652990 -0.215091 0.086 Uiso 1 1 calc R U . . . 
C4A C 0.6594(8) 0.6110(5) -0.382(3) 0.064(4) Uani 1 1 d . . . . . 
H4AA H 0.681976 0.620485 -0.503106 0.077 Uiso 1 1 calc R U . . . 
H4AB H 0.611108 0.617453 -0.386842 0.077 Uiso 1 1 calc R U . . . 
C5A C 0.7426(6) 0.5593(5) 0.0101(18) 0.043(3) Uani 1 1 d . . . . . 
C6A C 0.8007(6) 0.4983(5) 0.148(2) 0.051(3) Uani 1 1 d . . . . . 
H6A H 0.759033 0.495287 0.226538 0.061 Uiso 1 1 calc R U . . . 
C7A C 0.8196(6) 0.4533(5) 0.066(2) 0.049(3) Uani 1 1 d . . . . . 
C8A C 0.8005(7) 0.4400(6) -0.113(2) 0.065(4) Uani 1 1 d . . . . . 
H8A H 0.774753 0.459419 -0.191464 0.077 Uiso 1 1 calc R U . . . 
C9A C 0.8180(8) 0.3977(6) -0.187(3) 0.070(5) Uani 1 1 d . . . . . 
H9A H 0.806364 0.389020 -0.315471 0.084 Uiso 1 1 calc R U . . . 
C10A C 0.8525(8) 0.3699(6) -0.065(3) 0.070(5) Uani 1 1 d . . . . . 
C11A C 0.8717(8) 0.3816(6) 0.109(3) 0.070(5) Uani 1 1 d . . . . . 
H11A H 0.897048 0.361683 0.186683 0.084 Uiso 1 1 calc R U . . . 
C12A C 0.8546(7) 0.4240(6) 0.182(3) 0.066(4) Uani 1 1 d . . . . . 
H12A H 0.867238 0.432218 0.309985 0.079 Uiso 1 1 calc R U . . . 
C13A C 0.8548(6) 0.5193(5) 0.2732(19) 0.043(3) Uani 1 1 d . . . . . 
C14A C 0.8474(8) 0.5232(7) 0.468(2) 0.071(5) Uani 1 1 d . . . . . 
H14A H 0.806521 0.514266 0.525464 0.085 Uiso 1 1 calc R U . . . 
C15A C 0.8974(8) 0.5399(8) 0.588(2) 0.090(7) Uani 1 1 d . . . . . 
H15A H 0.891658 0.541323 0.724816 0.108 Uiso 1 1 calc R U . . . 
C16A C 0.9552(7) 0.5541(6) 0.501(2) 0.067(5) Uani 1 1 d . . . . . 
C17A C 0.9637(7) 0.5524(6) 0.307(3) 0.072(5) Uani 1 1 d . . . . . 
H17A H 1.003783 0.563316 0.251443 0.087 Uiso 1 1 calc R U . . . 
C18A C 0.9139(7) 0.5347(6) 0.185(2) 0.064(4) Uani 1 1 d . . . . . 
H18A H 0.919985 0.533145 0.047828 0.077 Uiso 1 1 calc R U . . . 
B1A B 0.6157(7) 0.5384(6) -0.2137(17) 0.044(4) Uani 1 1 d . . . . . 
Br1B Br 0.20060(12) 0.26001(12) 0.3470(8) 0.1713(18) Uani 1 1 d . . . . . 
Br2B Br 0.61634(13) 0.14434(9) 1.1287(6) 0.1418(14) Uani 1 1 d . . . . . 
F1B F 0.5397(4) 0.4518(3) 0.1556(10) 0.0512(19) Uani 1 1 d . . . . . 
F2B F 0.5034(4) 0.4084(3) 0.4044(10) 0.0514(19) Uani 1 1 d . . . . . 
F3B F 0.6029(4) 0.4436(3) 0.4211(11) 0.056(2) Uani 1 1 d . . . . . 
O1B O 0.5876(5) 0.3510(3) 0.6700(15) 0.057(2) Uani 1 1 d . . . . . 
O2B O 0.5300(5) 0.3026(3) 0.4851(15) 0.054(2) Uani 1 1 d . . . . . 
C1B C 0.5957(7) 0.3781(5) 0.194(2) 0.050(3) Uani 1 1 d . . . . . 
H1B H 0.570353 0.366610 0.079367 0.060 Uiso 1 1 calc R U . . . 
C2B C 0.6203(7) 0.3385(5) 0.338(2) 0.052(3) Uani 1 1 d . . . . . 
H2B H 0.623154 0.309805 0.265566 0.063 Uiso 1 1 calc R U . . . 
C3B C 0.6878(7) 0.3614(6) 0.343(3) 0.082(6) Uani 1 1 d . . . . . 
H3BA H 0.726001 0.340725 0.332550 0.098 Uiso 1 1 calc R U . . . 
H3BB H 0.693488 0.381978 0.453600 0.098 Uiso 1 1 calc R U . . . 
C4B C 0.6699(8) 0.3847(6) 0.148(3) 0.080(6) Uani 1 1 d . . . . . 
H4BA H 0.683719 0.416167 0.142784 0.097 Uiso 1 1 calc R U . . . 
H4BB H 0.685138 0.368418 0.031147 0.097 Uiso 1 1 calc R U . . . 
C5B C 0.5796(7) 0.3333(5) 0.518(3) 0.055(4) Uani 1 1 d . . . . . 
C6B C 0.4848(7) 0.2936(5) 0.647(2) 0.057(4) Uani 1 1 d . . . . . 
H6B H 0.481394 0.320614 0.730349 0.068 Uiso 1 1 calc R U . . . 
C7B C 0.4181(7) 0.2834(5) 0.564(2) 0.051(4) Uani 1 1 d . . . . . 
C8B C 0.3993(8) 0.2973(5) 0.381(3) 0.074(5) Uani 1 1 d . . . . . 
H8B H 0.431118 0.311201 0.298662 0.088 Uiso 1 1 calc R U . . . 
C9B C 0.3336(9) 0.2911(6) 0.313(3) 0.078(5) Uani 1 1 d . . . . . 
H9B H 0.320474 0.301096 0.187788 0.094 Uiso 1 1 calc R U . . . 
C10B C 0.2878(9) 0.2696(6) 0.439(4) 0.085(6) Uani 1 1 d . . . . . 
C11B C 0.3064(8) 0.2539(7) 0.623(4) 0.087(6) Uani 1 1 d . . . . . 
H11B H 0.276187 0.238663 0.706058 0.105 Uiso 1 1 calc R U . . . 
C12B C 0.3720(8) 0.2622(5) 0.677(3) 0.073(5) Uani 1 1 d . . . . . 
H12B H 0.385912 0.252347 0.802367 0.088 Uiso 1 1 calc R U . . . 
C13B C 0.5152(7) 0.2560(5) 0.765(2) 0.057(4) Uani 1 1 d . . . . . 
C14B C 0.5339(8) 0.2633(6) 0.951(3) 0.069(5) Uani 1 1 d . . . . . 
H14B H 0.526949 0.291913 1.004553 0.083 Uiso 1 1 calc R U . . . 
C15B C 0.5634(9) 0.2304(7) 1.069(3) 0.083(6) Uani 1 1 d . . . . . 
H15B H 0.575633 0.235926 1.200324 0.100 Uiso 1 1 calc R U . . . 
C16B C 0.5732(8) 0.1903(7) 0.983(4) 0.086(7) Uani 1 1 d . . . . . 
C17B C 0.5535(8) 0.1806(6) 0.798(4) 0.096(8) Uani 1 1 d . . . . . 
H17B H 0.559495 0.151632 0.746535 0.115 Uiso 1 1 calc R U . . . 
C18B C 0.5241(8) 0.2141(5) 0.682(3) 0.072(5) Uani 1 1 d . . . . . 
H18B H 0.510889 0.208398 0.551414 0.087 Uiso 1 1 calc R U . . . 
B1B B 0.5602(7) 0.4198(6) 0.291(2) 0.048(4) Uani 1 1 d . . . . . 
K1A K 0.59325(13) 0.53329(10) 0.2721(4) 0.0444(6) Uani 1 1 d . . . . . 
K1B K 0.55031(13) 0.43488(10) -0.2250(4) 0.0419(6) Uani 1 1 d . . . . . 
  
  
_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 
Br1A C10A 1.912(17) . ? 
Br2A C16A 1.887(15) . ? 
F1A B1A 1.414(15) . ? 
F1A K1A 2.678(8) 1_554 ? 
F1A K1B 2.804(8) . ? 
F1A K1B 2.821(8) 2_665 ? 
F2A B1A 1.429(17) . ? 
F2A K1B 2.779(8) . ? 
F2A K1A 2.867(8) . ? 
F3A B1A 1.417(16) . ? 
F3A K1A 2.674(8) . ? 
F3A K1B 2.768(7) 2_665 ? 
O1A C5A 1.184(15) . ? 
O1A K1A 2.741(9) . ? 
O2A C5A 1.353(16) . ? 
O2A C6A 1.439(17) . ? 
C1A C4A 1.55(2) . ? 
C1A C2A 1.566(16) . ? 
C1A B1A 1.596(18) . ? 
C2A C5A 1.503(18) . ? 
C2A C3A 1.538(19) . ? 
C3A C4A 1.54(2) . ? 
C6A C7A 1.51(2) . ? 
C6A C13A 1.525(17) . ? 
C7A C8A 1.35(2) . ? 
C7A C12A 1.38(2) . ? 
C8A C9A 1.42(2) . ? 
C9A C10A 1.37(2) . ? 
C10A C11A 1.30(3) . ? 
C11A C12A 1.41(2) . ? 
C13A C14A 1.35(2) . ? 
C13A C18A 1.410(18) . ? 
C14A C15A 1.39(2) . ? 
C15A C16A 1.37(2) . ? 
C16A C17A 1.34(2) . ? 
C17A C18A 1.41(2) . ? 
Br1B C10B 1.883(17) . ? 
Br2B C16B 1.913(19) . ? 
F1B B1B 1.402(17) . ? 
F1B K1B 2.671(8) . ? 
F1B K1A 2.800(8) . ? 
F1B K1A 2.822(8) 2_665 ? 
F2B B1B 1.423(14) . ? 
F2B K1A 2.771(8) 2_665 ? 
F2B K1B 2.828(8) 1_556 ? 
F3B B1B 1.431(17) . ? 
F3B K1B 2.662(8) 1_556 ? 
F3B K1A 2.898(9) . ? 
O1B C5B 1.183(18) . ? 
O1B K1B 2.736(11) 1_556 ? 
O2B C5B 1.379(17) . ? 
O2B C6B 1.459(18) . ? 
C1B C4B 1.535(19) . ? 
C1B B1B 1.59(2) . ? 
C1B C2B 1.63(2) . ? 
C2B C5B 1.49(2) . ? 
C2B C3B 1.520(19) . ? 
C3B C4B 1.55(3) . ? 
C6B C7B 1.49(2) . ? 
C6B C13B 1.52(2) . ? 
C7B C12B 1.37(2) . ? 
C7B C8B 1.38(2) . ? 
C8B C9B 1.41(2) . ? 
C9B C10B 1.42(3) . ? 
C10B C11B 1.40(3) . ? 
C11B C12B 1.39(2) . ? 
C13B C14B 1.34(2) . ? 
C13B C18B 1.40(2) . ? 
C14B C15B 1.41(2) . ? 
C15B C16B 1.36(3) . ? 
C16B C17B 1.37(3) . ? 
C17B C18B 1.41(3) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
B1A F1A K1A 117.7(6) . 1_554 ? 
B1A F1A K1B 101.8(8) . . ? 
K1A F1A K1B 115.4(3) 1_554 . ? 
B1A F1A K1B 103.1(7) . 2_665 ? 
K1A F1A K1B 113.5(3) 1_554 2_665 ? 
K1B F1A K1B 103.5(2) . 2_665 ? 
B1A F2A K1B 102.5(7) . . ? 
B1A F2A K1A 97.6(7) . . ? 
K1B F2A K1A 109.3(2) . . ? 
B1A F3A K1A 106.8(7) . . ? 
B1A F3A K1B 105.5(7) . 2_665 ? 
K1A F3A K1B 114.2(3) . 2_665 ? 
C5A O1A K1A 127.1(8) . . ? 
C5A O2A C6A 116.5(10) . . ? 
C4A C1A C2A 88.3(10) . . ? 
C4A C1A B1A 113.4(12) . . ? 
C2A C1A B1A 115.9(10) . . ? 
C5A C2A C3A 122.9(13) . . ? 
C5A C2A C1A 117.3(11) . . ? 
C3A C2A C1A 87.2(10) . . ? 
C4A C3A C2A 89.7(12) . . ? 
C3A C4A C1A 87.9(11) . . ? 
O1A C5A O2A 124.4(13) . . ? 
O1A C5A C2A 126.2(14) . . ? 
O2A C5A C2A 109.2(11) . . ? 
O2A C6A C7A 106.7(11) . . ? 
O2A C6A C13A 108.7(11) . . ? 
C7A C6A C13A 113.8(11) . . ? 
C8A C7A C12A 118.4(16) . . ? 
C8A C7A C6A 122.2(14) . . ? 
C12A C7A C6A 119.3(14) . . ? 
C7A C8A C9A 121.7(17) . . ? 
C10A C9A C8A 117.2(17) . . ? 
C11A C10A C9A 122.9(18) . . ? 
C11A C10A Br1A 120.5(15) . . ? 
C9A C10A Br1A 116.6(15) . . ? 
C10A C11A C12A 119.7(17) . . ? 
C7A C12A C11A 120.1(16) . . ? 
C14A C13A C18A 119.3(14) . . ? 
C14A C13A C6A 121.1(13) . . ? 
C18A C13A C6A 119.6(12) . . ? 
C13A C14A C15A 122.5(15) . . ? 
C16A C15A C14A 117.9(15) . . ? 
C17A C16A C15A 121.5(15) . . ? 
C17A C16A Br2A 117.9(13) . . ? 
C15A C16A Br2A 120.6(12) . . ? 
C16A C17A C18A 121.0(16) . . ? 
C17A C18A C13A 117.7(14) . . ? 
F1A B1A F3A 104.3(10) . . ? 
F1A B1A F2A 107.0(12) . . ? 
F3A B1A F2A 106.5(9) . . ? 
F1A B1A C1A 112.4(9) . . ? 
F3A B1A C1A 113.0(13) . . ? 
F2A B1A C1A 113.1(11) . . ? 
B1B F1B K1B 119.6(8) . . ? 
B1B F1B K1A 107.6(8) . . ? 
K1B F1B K1A 114.6(3) . . ? 
B1B F1B K1A 101.5(7) . 2_665 ? 
K1B F1B K1A 112.5(3) . 2_665 ? 
K1A F1B K1A 98.1(3) . 2_665 ? 
B1B F2B K1A 103.2(8) . 2_665 ? 
B1B F2B K1B 99.0(7) . 1_556 ? 
K1A F2B K1B 110.4(3) 2_665 1_556 ? 
B1B F3B K1B 106.4(7) . 1_556 ? 
B1B F3B K1A 102.1(8) . . ? 
K1B F3B K1A 112.9(3) 1_556 . ? 
C5B O1B K1B 127.7(10) . 1_556 ? 
C5B O2B C6B 116.7(12) . . ? 
C4B C1B B1B 114.8(13) . . ? 
C4B C1B C2B 85.7(12) . . ? 
B1B C1B C2B 117.5(11) . . ? 
C5B C2B C3B 121.2(15) . . ? 
C5B C2B C1B 114.5(11) . . ? 
C3B C2B C1B 87.2(12) . . ? 
C2B C3B C4B 88.9(14) . . ? 
C1B C4B C3B 89.4(13) . . ? 
O1B C5B O2B 123.1(15) . . ? 
O1B C5B C2B 127.6(14) . . ? 
O2B C5B C2B 109.3(13) . . ? 
O2B C6B C7B 107.8(12) . . ? 
O2B C6B C13B 107.2(11) . . ? 
C7B C6B C13B 114.4(13) . . ? 
C12B C7B C8B 118.5(15) . . ? 
C12B C7B C6B 119.0(15) . . ? 
C8B C7B C6B 122.3(15) . . ? 
C7B C8B C9B 121.1(18) . . ? 
C8B C9B C10B 117.8(19) . . ? 
C11B C10B C9B 122.0(17) . . ? 
C11B C10B Br1B 120.0(16) . . ? 
C9B C10B Br1B 117.9(17) . . ? 
C12B C11B C10B 116(2) . . ? 
C7B C12B C11B 125(2) . . ? 
C14B C13B C18B 120.1(17) . . ? 
C14B C13B C6B 119.7(15) . . ? 
C18B C13B C6B 120.2(15) . . ? 
C13B C14B C15B 123.1(19) . . ? 
C16B C15B C14B 116(2) . . ? 
C15B C16B C17B 123.4(19) . . ? 
C15B C16B Br2B 119.0(19) . . ? 
C17B C16B Br2B 117.6(18) . . ? 
C16B C17B C18B 120(2) . . ? 
C13B C18B C17B 118(2) . . ? 
F1B B1B F2B 107.0(11) . . ? 
F1B B1B F3B 104.1(12) . . ? 
F2B B1B F3B 105.0(10) . . ? 
F1B B1B C1B 113.4(11) . . ? 
F2B B1B C1B 113.5(12) . . ? 
F3B B1B C1B 113.0(12) . . ? 
F3A K1A F1A 157.2(3) . 1_556 ? 
F3A K1A O1A 72.3(3) . . ? 
F1A K1A O1A 119.3(3) 1_556 . ? 
F3A K1A F2B 89.5(2) . 2_665 ? 
F1A K1A F2B 67.8(2) 1_556 2_665 ? 
O1A K1A F2B 119.0(3) . 2_665 ? 
F3A K1A F1B 91.4(2) . . ? 
F1A K1A F1B 95.8(2) 1_556 . ? 
O1A K1A F1B 125.3(3) . . ? 
F2B K1A F1B 112.5(2) 2_665 . ? 
F3A K1A F1B 65.1(2) . 2_665 ? 
F1A K1A F1B 96.5(2) 1_556 2_665 ? 
O1A K1A F1B 134.5(3) . 2_665 ? 
F2B K1A F1B 47.9(2) 2_665 2_665 ? 
F1B K1A F1B 72.3(3) . 2_665 ? 
F3A K1A F2A 48.4(2) . . ? 
F1A K1A F2A 152.4(3) 1_556 . ? 
O1A K1A F2A 66.5(2) . . ? 
F2B K1A F2A 135.9(2) 2_665 . ? 
F1B K1A F2A 64.2(2) . . ? 
F1B K1A F2A 95.0(2) 2_665 . ? 
F3A K1A F3B 132.9(3) . . ? 
F1A K1A F3B 63.8(2) 1_556 . ? 
O1A K1A F3B 112.3(3) . . ? 
F2B K1A F3B 121.5(2) 2_665 . ? 
F1B K1A F3B 46.1(2) . . ? 
F1B K1A F3B 108.2(2) 2_665 . ? 
F2A K1A F3B 88.8(2) . . ? 
F3B K1B F1B 154.9(3) 1_554 . ? 
F3B K1B O1B 75.1(3) 1_554 1_554 ? 
F1B K1B O1B 117.1(3) . 1_554 ? 
F3B K1B F3A 133.3(2) 1_554 2_665 ? 
F1B K1B F3A 66.0(2) . 2_665 ? 
O1B K1B F3A 109.6(3) 1_554 2_665 ? 
F3B K1B F2A 87.9(2) 1_554 . ? 
F1B K1B F2A 67.1(2) . . ? 
O1B K1B F2A 125.2(3) 1_554 . ? 
F3A K1B F2A 119.3(3) 2_665 . ? 
F3B K1B F1A 65.3(2) 1_554 . ? 
F1B K1B F1A 97.1(2) . . ? 
O1B K1B F1A 139.6(3) 1_554 . ? 
F3A K1B F1A 103.5(2) 2_665 . ? 
F2A K1B F1A 48.3(2) . . ? 
F3B K1B F1A 90.8(2) 1_554 2_665 ? 
F1B K1B F1A 98.0(2) . 2_665 ? 
O1B K1B F1A 124.8(3) 1_554 2_665 ? 
F3A K1B F1A 47.1(2) 2_665 2_665 ? 
F2A K1B F1A 106.8(2) . 2_665 ? 
F1A K1B F1A 65.6(2) . 2_665 ? 
F3B K1B F2B 48.6(2) 1_554 1_554 ? 
F1B K1B F2B 155.2(2) . 1_554 ? 
O1B K1B F2B 66.0(3) 1_554 1_554 ? 
F3A K1B F2B 89.5(2) 2_665 1_554 ? 
F2A K1B F2B 133.5(2) . 1_554 ? 
F1A K1B F2B 92.2(2) . 1_554 ? 
F1A K1B F2B 65.1(2) 2_665 1_554 ? 
  
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 
C4A C1A C2A C5A 145.4(13) . . . . ? 
B1A C1A C2A C5A 30.1(17) . . . . ? 
C4A C1A C2A C3A 19.6(11) . . . . ? 
B1A C1A C2A C3A -95.8(14) . . . . ? 
C5A C2A C3A C4A -140.6(12) . . . . ? 
C1A C2A C3A C4A -19.7(11) . . . . ? 
C2A C3A C4A C1A 19.9(11) . . . . ? 
C2A C1A C4A C3A -19.6(11) . . . . ? 
B1A C1A C4A C3A 98.0(12) . . . . ? 
K1A O1A C5A O2A -92.7(13) . . . . ? 
K1A O1A C5A C2A 83.1(17) . . . . ? 
C6A O2A C5A O1A 1.6(18) . . . . ? 
C6A O2A C5A C2A -174.8(10) . . . . ? 
C3A C2A C5A O1A 17(2) . . . . ? 
C1A C2A C5A O1A -88.8(17) . . . . ? 
C3A C2A C5A O2A -167.0(11) . . . . ? 
C1A C2A C5A O2A 87.6(13) . . . . ? 
C5A O2A C6A C7A 149.8(10) . . . . ? 
C5A O2A C6A C13A -87.1(13) . . . . ? 
O2A C6A C7A C8A -24.0(17) . . . . ? 
C13A C6A C7A C8A -143.9(13) . . . . ? 
O2A C6A C7A C12A 159.3(11) . . . . ? 
C13A C6A C7A C12A 39.4(17) . . . . ? 
C12A C7A C8A C9A -3(2) . . . . ? 
C6A C7A C8A C9A -179.4(13) . . . . ? 
C7A C8A C9A C10A 3(2) . . . . ? 
C8A C9A C10A C11A -3(3) . . . . ? 
C8A C9A C10A Br1A -179.7(11) . . . . ? 
C9A C10A C11A C12A 3(3) . . . . ? 
Br1A C10A C11A C12A 179.1(11) . . . . ? 
C8A C7A C12A C11A 2(2) . . . . ? 
C6A C7A C12A C11A 178.9(13) . . . . ? 
C10A C11A C12A C7A -2(2) . . . . ? 
O2A C6A C13A C14A 131.7(15) . . . . ? 
C7A C6A C13A C14A -109.6(17) . . . . ? 
O2A C6A C13A C18A -48.9(17) . . . . ? 
C7A C6A C13A C18A 69.8(18) . . . . ? 
C18A C13A C14A C15A -3(3) . . . . ? 
C6A C13A C14A C15A 176.1(17) . . . . ? 
C13A C14A C15A C16A 2(3) . . . . ? 
C14A C15A C16A C17A 0(3) . . . . ? 
C14A C15A C16A Br2A -178.9(15) . . . . ? 
C15A C16A C17A C18A -2(3) . . . . ? 
Br2A C16A C17A C18A 177.5(13) . . . . ? 
C16A C17A C18A C13A 1(3) . . . . ? 
C14A C13A C18A C17A 2(2) . . . . ? 
C6A C13A C18A C17A -177.7(14) . . . . ? 
K1A F1A B1A F3A 126.7(7) 1_554 . . . ? 
K1B F1A B1A F3A -106.1(9) . . . . ? 
K1B F1A B1A F3A 0.9(11) 2_665 . . . ? 
K1A F1A B1A F2A -120.8(8) 1_554 . . . ? 
K1B F1A B1A F2A 6.4(10) . . . . ? 
K1B F1A B1A F2A 113.5(8) 2_665 . . . ? 
K1A F1A B1A C1A 3.9(16) 1_554 . . . ? 
K1B F1A B1A C1A 131.1(11) . . . . ? 
K1B F1A B1A C1A -121.9(11) 2_665 . . . ? 
K1A F3A B1A F1A 120.9(8) . . . . ? 
K1B F3A B1A F1A -1.0(11) 2_665 . . . ? 
K1A F3A B1A F2A 8.0(11) . . . . ? 
K1B F3A B1A F2A -113.9(8) 2_665 . . . ? 
K1A F3A B1A C1A -116.7(9) . . . . ? 
K1B F3A B1A C1A 121.4(9) 2_665 . . . ? 
K1B F2A B1A F1A -6.5(10) . . . . ? 
K1A F2A B1A F1A -118.2(8) . . . . ? 
K1B F2A B1A F3A 104.5(9) . . . . ? 
K1A F2A B1A F3A -7.2(10) . . . . ? 
K1B F2A B1A C1A -130.8(9) . . . . ? 
K1A F2A B1A C1A 117.5(9) . . . . ? 
C4A C1A B1A F1A 78.3(16) . . . . ? 
C2A C1A B1A F1A 178.4(11) . . . . ? 
C4A C1A B1A F3A -39.4(15) . . . . ? 
C2A C1A B1A F3A 60.7(15) . . . . ? 
C4A C1A B1A F2A -160.5(12) . . . . ? 
C2A C1A B1A F2A -60.4(15) . . . . ? 
C4B C1B C2B C5B 145.4(14) . . . . ? 
B1B C1B C2B C5B 29.6(17) . . . . ? 
C4B C1B C2B C3B 22.2(13) . . . . ? 
B1B C1B C2B C3B -93.6(14) . . . . ? 
C5B C2B C3B C4B -139.0(15) . . . . ? 
C1B C2B C3B C4B -21.9(12) . . . . ? 
B1B C1B C4B C3B 96.7(15) . . . . ? 
C2B C1B C4B C3B -21.7(12) . . . . ? 
C2B C3B C4B C1B 23.2(13) . . . . ? 
K1B O1B C5B O2B -101.6(16) 1_556 . . . ? 
K1B O1B C5B C2B 80.7(18) 1_556 . . . ? 
C6B O2B C5B O1B 2(2) . . . . ? 
C6B O2B C5B C2B -179.6(11) . . . . ? 
C3B C2B C5B O1B 13(2) . . . . ? 
C1B C2B C5B O1B -89.5(19) . . . . ? 
C3B C2B C5B O2B -165.2(14) . . . . ? 
C1B C2B C5B O2B 92.5(14) . . . . ? 
C5B O2B C6B C7B 147.1(12) . . . . ? 
C5B O2B C6B C13B -89.3(14) . . . . ? 
O2B C6B C7B C12B 162.2(13) . . . . ? 
C13B C6B C7B C12B 43.0(19) . . . . ? 
O2B C6B C7B C8B -22.4(19) . . . . ? 
C13B C6B C7B C8B -141.6(15) . . . . ? 
C12B C7B C8B C9B 2(2) . . . . ? 
C6B C7B C8B C9B -173.4(15) . . . . ? 
C7B C8B C9B C10B -1(3) . . . . ? 
C8B C9B C10B C11B -1(3) . . . . ? 
C8B C9B C10B Br1B -178.4(13) . . . . ? 
C9B C10B C11B C12B 2(3) . . . . ? 
Br1B C10B C11B C12B 179.2(14) . . . . ? 
C8B C7B C12B C11B -1(3) . . . . ? 
C6B C7B C12B C11B 174.5(17) . . . . ? 
C10B C11B C12B C7B -1(3) . . . . ? 
O2B C6B C13B C14B 116.4(15) . . . . ? 
C7B C6B C13B C14B -124.1(15) . . . . ? 
O2B C6B C13B C18B -63.2(17) . . . . ? 
C7B C6B C13B C18B 56.3(18) . . . . ? 
C18B C13B C14B C15B 1(2) . . . . ? 
C6B C13B C14B C15B -179.0(14) . . . . ? 
C13B C14B C15B C16B 1(3) . . . . ? 
C14B C15B C16B C17B -3(3) . . . . ? 
C14B C15B C16B Br2B 177.4(12) . . . . ? 
C15B C16B C17B C18B 3(3) . . . . ? 
Br2B C16B C17B C18B -177.2(12) . . . . ? 
C14B C13B C18B C17B 0(2) . . . . ? 
C6B C13B C18B C17B 179.1(14) . . . . ? 
C16B C17B C18B C13B -1(2) . . . . ? 
K1B F1B B1B F2B -119.4(9) . . . . ? 
K1A F1B B1B F2B 107.5(10) . . . . ? 
K1A F1B B1B F2B 5.0(12) 2_665 . . . ? 
K1B F1B B1B F3B 129.7(8) . . . . ? 
K1A F1B B1B F3B -3.3(10) . . . . ? 
K1A F1B B1B F3B -105.8(8) 2_665 . . . ? 
K1B F1B B1B C1B 6.5(14) . . . . ? 
K1A F1B B1B C1B -126.5(10) . . . . ? 
K1A F1B B1B C1B 130.9(9) 2_665 . . . ? 
K1A F2B B1B F1B -5.1(12) 2_665 . . . ? 
K1B F2B B1B F1B -118.7(10) 1_556 . . . ? 
K1A F2B B1B F3B 105.1(10) 2_665 . . . ? 
K1B F2B B1B F3B -8.5(11) 1_556 . . . ? 
K1A F2B B1B C1B -131.0(10) 2_665 . . . ? 
K1B F2B B1B C1B 115.4(10) 1_556 . . . ? 
K1B F3B B1B F1B 121.7(8) 1_556 . . . ? 
K1A F3B B1B F1B 3.2(10) . . . . ? 
K1B F3B B1B F2B 9.3(12) 1_556 . . . ? 
K1A F3B B1B F2B -109.2(10) . . . . ? 
K1B F3B B1B C1B -114.9(9) 1_556 . . . ? 
K1A F3B B1B C1B 126.6(9) . . . . ? 
C4B C1B B1B F1B 82.7(17) . . . . ? 
C2B C1B B1B F1B -178.9(11) . . . . ? 
C4B C1B B1B F2B -154.9(14) . . . . ? 
C2B C1B B1B F2B -56.5(16) . . . . ? 
C4B C1B B1B F3B -35.5(18) . . . . ? 
C2B C1B B1B F3B 63.0(15) . . . . ? 
  
_refine_diff_density_max    0.692 
_refine_diff_density_min   -0.777 
_refine_diff_density_rms    0.105 
  
  
  
