data_caacbc6f5
_audit_creation_date 2015-02-02
_audit_creation_method
;
Olex2 1.2-ac2
(compiled Nov 7 2012 10:34:12, GUI svn.r4372)
;
_publ_contact_author_address ?
_publ_contact_author_email ?
_publ_contact_author_name ''
_publ_contact_author_phone ?
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C18 H B F15 O, C20 H32 N'
_chemical_formula_sum 'C38 H33 B F15 N O'
_chemical_formula_weight 815.46
_chemical_melting_point ?
_chemical_oxdiff_formula 'C H N O F B'
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'
'B' 'B' 0.0013 0.0007 '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'
'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060 '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/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'
_cell_length_a 11.2760(3)
_cell_length_b 18.8351(5)
_cell_length_c 17.0893(5)
_cell_angle_alpha 90.00
_cell_angle_beta 100.348(3)
_cell_angle_gamma 90.00
_cell_volume 3570.46(17)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 7498
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 26.3400
_cell_measurement_theta_min 2.1340
_exptl_absorpt_coefficient_mu 0.144
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.77575
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour 'metallic whitish colourless'
_exptl_crystal_colour_lustre metallic
_exptl_crystal_colour_modifier whitish
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.517
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1664
_exptl_crystal_size_max 0.64
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.15
_exptl_special_details
;
?
;
_diffrn_reflns_av_R_equivalents 0.0324
_diffrn_reflns_av_unetI/netI 0.0426
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 13899
_diffrn_reflns_theta_full 26.37
_diffrn_reflns_theta_max 26.37
_diffrn_reflns_theta_min 1.62
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type Eos
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9995
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega 43.00 119.00 1.0000 100.4000
omega____ theta____ kappa____ phi______frames
- 27.5074 178.0000 -180.0000 76
#__ type_ start__ end____ width___ exp.time_
2 omega -58.00 75.00 1.0000 100.4000
omega____ theta____ kappa____ phi______frames
- 27.5074 -19.0000 -180.0000 133
#__ type_ start__ end____ width___ exp.time_
3 omega 6.00 63.00 1.0000 100.4000
omega____ theta____ kappa____ phi______frames
- 27.5074 -57.0000 -90.0000 57
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0412813000
_diffrn_orient_matrix_UB_12 -0.0247143000
_diffrn_orient_matrix_UB_13 -0.0210953000
_diffrn_orient_matrix_UB_21 -0.0082541000
_diffrn_orient_matrix_UB_22 -0.0154336000
_diffrn_orient_matrix_UB_23 0.0365215000
_diffrn_orient_matrix_UB_31 -0.0481137000
_diffrn_orient_matrix_UB_32 0.0238335000
_diffrn_orient_matrix_UB_33 0.0017800000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_reflns_number_gt 6330
_reflns_number_total 7305
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_reflns_threshold_expression >2sigma(I)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max 0.389
_refine_diff_density_min -0.290
_refine_diff_density_rms 0.063
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.071
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 517
_refine_ls_number_reflns 7305
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0491
_refine_ls_R_factor_gt 0.0419
_refine_ls_restrained_S_all 1.071
_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^)+(0.0496P)^2^+2.0791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1115
_refine_ls_wR_factor_ref 0.1165
_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:
{H3A,H3B} of C3, H12 of C12, H18 of C18, H11 of C11, H13 of C13, H15 of C15,
H1 of C1
At 1.5 times of:
{H17A,H17B,H17C} of C17, {H6A,H6B,H6C} of C6, {H5A,H5B,H5C} of C5, {H19A,
H19B,H19C} of C19, {H20A,H20B,H20C} of C20, {H8A,H8B,H8C} of C8, {H16A,H16B,
H16C} of C16, {H7A,H7B,H7C} of C7
2.a Ternary CH refined with riding coordinates:
C18(H18), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
C11(H11), C13(H13), C12(H12), C1(H1)
2.d Idealised Me refined as rotating group:
C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C19(H19A,H19B,H19C), C7(H7A,H7B,H7C),
C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.87547(9) 0.18428(5) 0.90098(6) 0.0205(2) Uani 1 1 d . . .
F15 F 1.04742(9) -0.02562(6) 0.84652(6) 0.0211(2) Uani 1 1 d . . .
F11 F 0.67710(8) 0.09339(6) 0.85201(6) 0.0204(2) Uani 1 1 d . . .
F14 F 1.00840(10) -0.10705(6) 0.96591(6) 0.0249(2) Uani 1 1 d . . .
F5 F 0.77979(9) 0.16834(6) 0.61981(6) 0.0220(2) Uani 1 1 d . . .
F10 F 0.65672(8) 0.05020(6) 0.69641(7) 0.0231(2) Uani 1 1 d . . .
F4 F 0.71483(10) 0.30299(6) 0.61317(7) 0.0250(2) Uani 1 1 d . . .
F3 F 0.72166(9) 0.38035(5) 0.74818(7) 0.0247(3) Uani 1 1 d . . .
F12 F 0.63863(9) 0.00784(6) 0.96817(7) 0.0269(3) Uani 1 1 d . . .
O1 O 1.02855(10) 0.11091(7) 0.78635(8) 0.0187(3) Uani 1 1 d . . .
F2 F 0.79858(10) 0.31785(6) 0.89226(7) 0.0267(3) Uani 1 1 d . . .
F7 F 0.99267(11) -0.06157(6) 0.54249(7) 0.0303(3) Uani 1 1 d . . .
F6 F 1.06464(9) 0.01931(6) 0.66857(7) 0.0262(3) Uani 1 1 d . . .
F8 F 0.75552(11) -0.08636(6) 0.48831(7) 0.0323(3) Uani 1 1 d . . .
F13 F 0.80306(11) -0.09309(6) 1.02758(7) 0.0299(3) Uani 1 1 d . . .
F9 F 0.58757(10) -0.02982(7) 0.56740(7) 0.0295(3) Uani 1 1 d . . .
C21 C 0.83225(14) 0.16802(9) 0.76144(10) 0.0146(3) Uani 1 1 d . . .
C33 C 0.86614(14) 0.04028(9) 0.84334(10) 0.0146(3) Uani 1 1 d . . .
C32 C 0.74385(15) 0.02388(9) 0.65899(11) 0.0170(4) Uani 1 1 d . . .
C35 C 0.74095(15) 0.00091(10) 0.93851(11) 0.0193(4) Uani 1 1 d . . .
C23 C 0.79568(15) 0.28031(10) 0.82528(11) 0.0189(4) Uani 1 1 d . . .
B1 B 0.90016(16) 0.09020(10) 0.76996(12) 0.0143(4) Uani 1 1 d . . .
C38 C 0.94435(14) -0.01344(9) 0.87594(10) 0.0157(3) Uani 1 1 d . . .
C29 C 0.90961(17) -0.03231(10) 0.58013(11) 0.0212(4) Uani 1 1 d . . .
C37 C 0.92684(16) -0.05757(9) 0.93719(11) 0.0185(4) Uani 1 1 d . . .
C34 C 0.76362(14) 0.04445(9) 0.87738(10) 0.0156(3) Uani 1 1 d . . .
C22 C 0.83398(14) 0.21051(9) 0.82781(11) 0.0161(3) Uani 1 1 d . . .
C36 C 0.82329(17) -0.05017(9) 0.96886(11) 0.0200(4) Uani 1 1 d . . .
C24 C 0.75614(15) 0.31194(9) 0.75247(12) 0.0186(4) Uani 1 1 d . . .
C27 C 0.86385(14) 0.04058(9) 0.68935(10) 0.0152(3) Uani 1 1 d . . .
C26 C 0.78851(14) 0.20230(9) 0.69015(11) 0.0161(3) Uani 1 1 d . . .
C31 C 0.70538(16) -0.01697(10) 0.59313(11) 0.0206(4) Uani 1 1 d . . .
C25 C 0.75247(15) 0.27276(10) 0.68455(11) 0.0183(4) Uani 1 1 d . . .
C28 C 0.94405(15) 0.00997(9) 0.64635(11) 0.0181(4) Uani 1 1 d . . .
C30 C 0.78969(17) -0.04551(10) 0.55273(11) 0.0217(4) Uani 1 1 d . . .
N1 N 0.76796(12) 0.24430(8) 0.24585(9) 0.0146(3) Uani 1 1 d . . .
C10 C 0.64108(14) 0.15565(9) 0.29615(11) 0.0166(3) Uani 1 1 d . . .
C11 C 0.55023(15) 0.10477(10) 0.27998(12) 0.0209(4) Uani 1 1 d . . .
H11 H 0.5289 0.0789 0.3217 0.025 Uiso 1 1 calc R . .
C18 C 0.69736(15) 0.17192(10) 0.38199(11) 0.0192(4) Uani 1 1 d . . .
H18 H 0.7725 0.1979 0.3816 0.023 Uiso 1 1 calc R . .
C13 C 0.51915(15) 0.13130(10) 0.14056(11) 0.0214(4) Uani 1 1 d . . .
H13 H 0.4777 0.1227 0.0893 0.026 Uiso 1 1 calc R . .
C14 C 0.60832(15) 0.18356(9) 0.15281(11) 0.0172(4) Uani 1 1 d . . .
C15 C 0.62616(16) 0.23055(10) 0.08359(11) 0.0213(4) Uani 1 1 d . . .
H15 H 0.6978 0.2598 0.1012 0.026 Uiso 1 1 calc R . .
C9 C 0.67038(14) 0.19244(9) 0.23090(11) 0.0158(3) Uani 1 1 d . . .
C3 C 0.96158(15) 0.29578(10) 0.27876(11) 0.0188(4) Uani 1 1 d . . .
H3A H 1.0242 0.3092 0.2494 0.023 Uiso 1 1 calc R . .
H3B H 0.9979 0.2898 0.3343 0.023 Uiso 1 1 calc R . .
C12 C 0.49135(16) 0.09207(10) 0.20327(12) 0.0229(4) Uani 1 1 d . . .
H12 H 0.4326 0.0569 0.1937 0.027 Uiso 1 1 calc R . .
C4 C 0.90127(14) 0.22629(10) 0.24536(11) 0.0176(4) Uani 1 1 d . . .
C5 C 0.94031(16) 0.16197(11) 0.29674(14) 0.0276(4) Uani 1 1 d . . .
H5A H 0.9375 0.1729 0.3512 0.041 Uiso 1 1 calc R . .
H5B H 1.0211 0.1492 0.2920 0.041 Uiso 1 1 calc R . .
H5C H 0.8871 0.1230 0.2796 0.041 Uiso 1 1 calc R . .
C6 C 0.91585(16) 0.21092(11) 0.16021(12) 0.0247(4) Uani 1 1 d . . .
H6A H 0.8647 0.1720 0.1397 0.037 Uiso 1 1 calc R . .
H6B H 0.9983 0.1989 0.1592 0.037 Uiso 1 1 calc R . .
H6C H 0.8938 0.2522 0.1280 0.037 Uiso 1 1 calc R . .
C19 C 0.61389(18) 0.22006(12) 0.41982(12) 0.0284(4) Uani 1 1 d . . .
H19A H 0.5963 0.2622 0.3883 0.043 Uiso 1 1 calc R . .
H19B H 0.6528 0.2328 0.4726 0.043 Uiso 1 1 calc R . .
H19C H 0.5402 0.1953 0.4223 0.043 Uiso 1 1 calc R . .
C1 C 0.75077(14) 0.31010(9) 0.25788(10) 0.0162(3) Uani 1 1 d . . .
H1 H 0.6749 0.3291 0.2588 0.019 Uiso 1 1 calc R . .
C7 C 0.86080(17) 0.40166(11) 0.19747(13) 0.0283(4) Uani 1 1 d . . .
H7A H 0.9322 0.4305 0.2050 0.042 Uiso 1 1 calc R . .
H7B H 0.7909 0.4317 0.1909 0.042 Uiso 1 1 calc R . .
H7C H 0.8580 0.3727 0.1509 0.042 Uiso 1 1 calc R . .
C2 C 0.86290(14) 0.35392(10) 0.27026(11) 0.0185(4) Uani 1 1 d . . .
C20 C 0.72844(17) 0.10474(11) 0.43098(12) 0.0254(4) Uani 1 1 d . . .
H20A H 0.6555 0.0815 0.4385 0.038 Uiso 1 1 calc R . .
H20B H 0.7753 0.1169 0.4818 0.038 Uiso 1 1 calc R . .
H20C H 0.7741 0.0734 0.4035 0.038 Uiso 1 1 calc R . .
C8 C 0.87024(16) 0.39927(11) 0.34533(13) 0.0287(5) Uani 1 1 d . . .
H8A H 0.8615 0.3694 0.3895 0.043 Uiso 1 1 calc R . .
H8B H 0.8069 0.4340 0.3373 0.043 Uiso 1 1 calc R . .
H8C H 0.9469 0.4229 0.3563 0.043 Uiso 1 1 calc R . .
C16 C 0.51788(18) 0.28045(12) 0.06227(14) 0.0327(5) Uani 1 1 d . . .
H16A H 0.4459 0.2529 0.0464 0.049 Uiso 1 1 calc R . .
H16B H 0.5297 0.3109 0.0193 0.049 Uiso 1 1 calc R . .
H16C H 0.5102 0.3088 0.1078 0.049 Uiso 1 1 calc R . .
C17 C 0.64705(19) 0.18812(13) 0.01096(12) 0.0316(5) Uani 1 1 d . . .
H17A H 0.7144 0.1568 0.0260 0.047 Uiso 1 1 calc R . .
H17B H 0.6635 0.2201 -0.0295 0.047 Uiso 1 1 calc R . .
H17C H 0.5763 0.1608 -0.0093 0.047 Uiso 1 1 calc R . .
H1A H 1.075(3) 0.0759(17) 0.7966(19) 0.059(9) Uiso 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
F1 0.0277(5) 0.0173(5) 0.0152(5) 0.0006(4) 0.0004(4) 0.0005(4)
F15 0.0208(5) 0.0193(5) 0.0244(6) 0.0038(5) 0.0070(4) 0.0063(4)
F11 0.0151(5) 0.0217(5) 0.0250(6) 0.0032(5) 0.0054(4) 0.0029(4)
F14 0.0364(6) 0.0174(5) 0.0197(6) 0.0047(5) 0.0015(4) 0.0086(4)
F5 0.0334(6) 0.0169(5) 0.0153(5) 0.0000(4) 0.0030(4) 0.0040(4)
F10 0.0144(5) 0.0308(6) 0.0247(6) -0.0039(5) 0.0050(4) -0.0011(4)
F4 0.0324(6) 0.0185(5) 0.0224(6) 0.0070(5) 0.0000(4) 0.0059(4)
F3 0.0280(5) 0.0117(5) 0.0341(7) 0.0013(5) 0.0049(5) 0.0057(4)
F12 0.0256(5) 0.0300(6) 0.0286(6) 0.0023(5) 0.0144(5) -0.0039(5)
O1 0.0139(6) 0.0150(6) 0.0266(7) 0.0021(5) 0.0020(5) -0.0007(5)
F2 0.0383(6) 0.0178(5) 0.0242(6) -0.0064(5) 0.0059(5) 0.0036(5)
F7 0.0407(6) 0.0253(6) 0.0289(7) -0.0026(5) 0.0175(5) 0.0088(5)
F6 0.0170(5) 0.0298(6) 0.0335(7) -0.0029(5) 0.0086(4) 0.0044(4)
F8 0.0500(7) 0.0273(6) 0.0187(6) -0.0063(5) 0.0035(5) -0.0052(5)
F13 0.0460(7) 0.0243(6) 0.0219(6) 0.0072(5) 0.0126(5) -0.0019(5)
F9 0.0244(5) 0.0366(7) 0.0248(6) -0.0018(5) -0.0033(4) -0.0097(5)
C21 0.0114(7) 0.0137(8) 0.0188(9) 0.0020(7) 0.0031(6) -0.0003(6)
C33 0.0165(8) 0.0121(8) 0.0141(8) -0.0017(7) -0.0005(6) -0.0029(6)
C32 0.0193(8) 0.0150(8) 0.0178(9) 0.0029(7) 0.0059(7) 0.0014(6)
C35 0.0198(8) 0.0206(9) 0.0186(9) -0.0051(8) 0.0062(7) -0.0055(7)
C23 0.0184(8) 0.0161(9) 0.0224(10) -0.0041(7) 0.0046(7) -0.0006(6)
B1 0.0130(8) 0.0130(9) 0.0169(10) 0.0025(8) 0.0029(7) 0.0010(7)
C38 0.0170(8) 0.0140(8) 0.0156(9) -0.0034(7) 0.0013(6) -0.0013(6)
C29 0.0310(9) 0.0153(9) 0.0200(10) 0.0042(7) 0.0115(7) 0.0061(7)
C37 0.0258(9) 0.0119(8) 0.0156(9) -0.0015(7) -0.0024(7) 0.0010(7)
C34 0.0160(8) 0.0124(8) 0.0169(9) -0.0012(7) -0.0015(6) -0.0004(6)
C22 0.0144(7) 0.0153(8) 0.0179(9) 0.0022(7) 0.0014(6) -0.0005(6)
C36 0.0327(9) 0.0145(8) 0.0124(9) 0.0008(7) 0.0029(7) -0.0058(7)
C24 0.0163(8) 0.0110(8) 0.0287(10) 0.0012(7) 0.0045(7) 0.0026(6)
C27 0.0179(8) 0.0121(8) 0.0158(9) 0.0041(7) 0.0038(6) 0.0004(6)
C26 0.0150(7) 0.0158(8) 0.0177(9) -0.0011(7) 0.0032(6) -0.0001(6)
C31 0.0220(8) 0.0199(9) 0.0184(9) 0.0049(8) -0.0006(7) -0.0048(7)
C25 0.0165(8) 0.0173(9) 0.0203(9) 0.0055(7) 0.0012(6) 0.0014(6)
C28 0.0184(8) 0.0157(8) 0.0208(9) 0.0048(7) 0.0049(7) 0.0017(6)
C30 0.0370(10) 0.0144(9) 0.0131(9) 0.0007(7) 0.0027(7) -0.0022(7)
N1 0.0124(6) 0.0161(7) 0.0155(7) -0.0006(6) 0.0035(5) -0.0001(5)
C10 0.0151(7) 0.0161(8) 0.0185(9) -0.0006(7) 0.0025(6) 0.0023(6)
C11 0.0216(8) 0.0180(9) 0.0236(10) 0.0034(8) 0.0057(7) -0.0021(7)
C18 0.0172(8) 0.0233(9) 0.0168(9) 0.0001(8) 0.0023(6) -0.0013(7)
C13 0.0206(8) 0.0212(9) 0.0206(10) -0.0041(8) -0.0012(7) -0.0031(7)
C14 0.0168(8) 0.0156(8) 0.0194(9) -0.0010(7) 0.0035(7) 0.0012(6)
C15 0.0197(8) 0.0259(10) 0.0178(9) 0.0023(8) 0.0024(7) -0.0019(7)
C9 0.0126(7) 0.0137(8) 0.0211(9) -0.0023(7) 0.0036(6) -0.0001(6)
C3 0.0135(7) 0.0212(9) 0.0215(10) -0.0017(8) 0.0029(6) 0.0003(7)
C12 0.0211(8) 0.0190(9) 0.0277(10) -0.0029(8) 0.0020(7) -0.0061(7)
C4 0.0108(7) 0.0198(9) 0.0226(9) -0.0014(8) 0.0042(6) 0.0008(6)
C5 0.0185(8) 0.0240(10) 0.0413(12) 0.0069(9) 0.0076(8) 0.0064(7)
C6 0.0180(8) 0.0303(11) 0.0269(11) -0.0102(9) 0.0072(7) 0.0003(7)
C19 0.0288(10) 0.0343(11) 0.0212(10) -0.0038(9) 0.0019(8) 0.0083(8)
C1 0.0152(7) 0.0184(9) 0.0152(9) -0.0012(7) 0.0034(6) 0.0006(6)
C7 0.0221(9) 0.0237(10) 0.0397(12) 0.0087(9) 0.0073(8) -0.0010(7)
C2 0.0140(8) 0.0173(9) 0.0245(10) -0.0034(8) 0.0042(7) -0.0009(6)
C20 0.0265(9) 0.0273(10) 0.0213(10) 0.0035(8) 0.0014(7) 0.0021(8)
C8 0.0177(8) 0.0303(11) 0.0377(12) -0.0160(10) 0.0041(8) -0.0028(7)
C16 0.0273(10) 0.0311(11) 0.0383(13) 0.0156(10) 0.0021(9) 0.0015(8)
C17 0.0347(11) 0.0425(13) 0.0181(10) -0.0029(9) 0.0060(8) -0.0062(9)
_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
F1 C22 1.348(2) . ?
F15 C38 1.3660(19) . ?
F11 C34 1.3555(19) . ?
F14 C37 1.339(2) . ?
F5 C26 1.350(2) . ?
F10 C32 1.3585(19) . ?
F4 C25 1.344(2) . ?
F3 C24 1.344(2) . ?
F12 C35 1.347(2) . ?
O1 B1 1.477(2) . ?
F2 C23 1.341(2) . ?
F7 C29 1.346(2) . ?
F6 C28 1.356(2) . ?
F8 C30 1.342(2) . ?
F13 C36 1.340(2) . ?
F9 C31 1.344(2) . ?
C21 B1 1.648(2) . ?
C21 C22 1.385(3) . ?
C21 C26 1.389(2) . ?
C33 B1 1.666(3) . ?
C33 C38 1.391(2) . ?
C33 C34 1.387(2) . ?
C32 C27 1.395(2) . ?
C32 C31 1.368(3) . ?
C35 C34 1.387(3) . ?
C35 C36 1.373(3) . ?
C23 C22 1.382(2) . ?
C23 C24 1.379(3) . ?
B1 C27 1.654(3) . ?
C38 C37 1.378(3) . ?
C29 C28 1.381(3) . ?
C29 C30 1.372(3) . ?
C37 C36 1.379(3) . ?
C24 C25 1.370(3) . ?
C27 C28 1.389(2) . ?
C26 C25 1.386(2) . ?
C31 C30 1.380(3) . ?
N1 C9 1.459(2) . ?
N1 C4 1.5425(19) . ?
N1 C1 1.277(2) . ?
C10 C11 1.394(2) . ?
C10 C18 1.521(2) . ?
C10 C9 1.402(3) . ?
C11 C12 1.380(3) . ?
C18 C19 1.531(3) . ?
C18 C20 1.523(3) . ?
C13 C14 1.396(2) . ?
C13 C12 1.383(3) . ?
C14 C15 1.519(3) . ?
C14 C9 1.401(2) . ?
C15 C16 1.532(3) . ?
C15 C17 1.530(3) . ?
C3 C4 1.537(2) . ?
C3 C2 1.549(2) . ?
C4 C5 1.514(3) . ?
C4 C6 1.521(3) . ?
C1 C2 1.493(2) . ?
C7 C2 1.532(3) . ?
C2 C8 1.531(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
C22 C21 B1 120.23(15) . . ?
C22 C21 C26 113.60(15) . . ?
C26 C21 B1 125.25(16) . . ?
C38 C33 B1 119.79(14) . . ?
C34 C33 B1 127.28(15) . . ?
C34 C33 C38 112.92(16) . . ?
F10 C32 C27 118.54(16) . . ?
F10 C32 C31 116.31(15) . . ?
C31 C32 C27 125.15(16) . . ?
F12 C35 C34 120.79(16) . . ?
F12 C35 C36 119.51(16) . . ?
C36 C35 C34 119.69(16) . . ?
F2 C23 C22 121.02(17) . . ?
F2 C23 C24 119.78(16) . . ?
C24 C23 C22 119.18(17) . . ?
O1 B1 C21 101.89(13) . . ?
O1 B1 C33 110.89(14) . . ?
O1 B1 C27 113.25(14) . . ?
C21 B1 C33 113.72(14) . . ?
C21 B1 C27 112.79(14) . . ?
C27 B1 C33 104.59(13) . . ?
F15 C38 C33 119.65(15) . . ?
F15 C38 C37 115.20(15) . . ?
C37 C38 C33 125.15(16) . . ?
F7 C29 C28 120.68(17) . . ?
F7 C29 C30 119.38(17) . . ?
C30 C29 C28 119.94(16) . . ?
F14 C37 C38 121.03(16) . . ?
F14 C37 C36 120.03(16) . . ?
C38 C37 C36 118.95(16) . . ?
F11 C34 C33 120.72(15) . . ?
F11 C34 C35 115.05(15) . . ?
C33 C34 C35 124.24(16) . . ?
F1 C22 C21 119.96(15) . . ?
F1 C22 C23 115.61(16) . . ?
C23 C22 C21 124.44(17) . . ?
F13 C36 C35 120.76(17) . . ?
F13 C36 C37 120.20(16) . . ?
C35 C36 C37 119.03(17) . . ?
F3 C24 C23 120.44(17) . . ?
F3 C24 C25 120.38(16) . . ?
C25 C24 C23 119.17(16) . . ?
C32 C27 B1 121.02(15) . . ?
C28 C27 C32 112.95(16) . . ?
C28 C27 B1 126.01(15) . . ?
F5 C26 C21 121.25(15) . . ?
F5 C26 C25 114.75(15) . . ?
C25 C26 C21 124.00(17) . . ?
F9 C31 C32 121.27(17) . . ?
F9 C31 C30 119.68(17) . . ?
C32 C31 C30 119.04(16) . . ?
F4 C25 C24 119.83(16) . . ?
F4 C25 C26 120.61(17) . . ?
C24 C25 C26 119.57(17) . . ?
F6 C28 C29 115.12(15) . . ?
F6 C28 C27 120.90(16) . . ?
C29 C28 C27 123.97(16) . . ?
F8 C30 C29 120.28(17) . . ?
F8 C30 C31 120.78(17) . . ?
C29 C30 C31 118.94(17) . . ?
C9 N1 C4 123.83(13) . . ?
C1 N1 C9 123.12(14) . . ?
C1 N1 C4 113.00(14) . . ?
C11 C10 C18 119.61(16) . . ?
C11 C10 C9 116.87(16) . . ?
C9 C10 C18 123.40(15) . . ?
C12 C11 C10 121.25(17) . . ?
C10 C18 C19 110.17(14) . . ?
C10 C18 C20 112.19(16) . . ?
C20 C18 C19 110.99(16) . . ?
C12 C13 C14 121.19(17) . . ?
C13 C14 C15 119.12(16) . . ?
C13 C14 C9 116.75(16) . . ?
C9 C14 C15 123.97(15) . . ?
C14 C15 C16 109.33(15) . . ?
C14 C15 C17 112.87(17) . . ?
C17 C15 C16 111.10(17) . . ?
C10 C9 N1 118.02(15) . . ?
C14 C9 N1 118.59(15) . . ?
C14 C9 C10 123.36(15) . . ?
C4 C3 C2 107.74(13) . . ?
C11 C12 C13 120.40(17) . . ?
C3 C4 N1 100.21(13) . . ?
C5 C4 N1 110.78(14) . . ?
C5 C4 C3 113.76(15) . . ?
C5 C4 C6 109.40(16) . . ?
C6 C4 N1 108.66(14) . . ?
C6 C4 C3 113.62(15) . . ?
N1 C1 C2 114.22(14) . . ?
C1 C2 C3 101.44(14) . . ?
C1 C2 C7 108.68(15) . . ?
C1 C2 C8 110.13(15) . . ?
C7 C2 C3 113.40(15) . . ?
C8 C2 C3 112.70(15) . . ?
C8 C2 C7 110.10(16) . . ?