static-content.springer.com10.1007... · web view1 omega 150.00 178.00 1.0000 2.9900 omega____...

data_3

_audit_creation_date 2015-02-02

_audit_creation_method

;

Olex2 1.2-ac2

(compiled 2012.03.27 svn.r2268, GUI svn.r4156)

;

_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 'C H2 Cl2, C38 H31 B F15 N'

_chemical_formula_sum 'C39 H33 B Cl2 F15 N'

_chemical_formula_weight 882.37

_chemical_melting_point ?

_chemical_oxdiff_formula 'C H N B F'

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'

'Cl' 'Cl' 0.3639 0.7018 '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'

'N' 'N' 0.0311 0.0180 '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 10.6273(2)

_cell_length_b 19.7950(5)

_cell_length_c 17.5470(4)

_cell_angle_alpha 90.00

_cell_angle_beta 95.180(2)

_cell_angle_gamma 90.00

_cell_volume 3676.23(14)

_cell_formula_units_Z 4

_cell_measurement_reflns_used 8343

_cell_measurement_temperature 100.01(10)

_cell_measurement_theta_max 65.4360

_cell_measurement_theta_min 2.5330

_exptl_absorpt_coefficient_mu 2.578

_exptl_absorpt_correction_T_max 1.00000

_exptl_absorpt_correction_T_min 0.68538

_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 'clear light colourless'

_exptl_crystal_colour_lustre clear

_exptl_crystal_colour_modifier light

_exptl_crystal_colour_primary colourless

_exptl_crystal_density_diffrn 1.594

_exptl_crystal_density_meas ?

_exptl_crystal_density_method 'not measured'

_exptl_crystal_description block

_exptl_crystal_F_000 1792

_exptl_crystal_size_max 0.63

_exptl_crystal_size_mid 0.21

_exptl_crystal_size_min 0.16

_exptl_special_details

;

?

;

_diffrn_reflns_av_R_equivalents 0.0514

_diffrn_reflns_av_unetI/netI 0.0497

_diffrn_reflns_limit_h_max 12

_diffrn_reflns_limit_h_min -12

_diffrn_reflns_limit_k_max 23

_diffrn_reflns_limit_k_min -23

_diffrn_reflns_limit_l_max 20

_diffrn_reflns_limit_l_min -14

_diffrn_reflns_number 15364

_diffrn_reflns_theta_full 65.39

_diffrn_reflns_theta_max 65.39

_diffrn_reflns_theta_min 3.37

_diffrn_ambient_environment N~2~

_diffrn_ambient_temperature 100.01(10)

_diffrn_detector 'CCD plate'

_diffrn_detector_area_resol_mean 7.9580

_diffrn_detector_type Eos

_diffrn_measured_fraction_theta_full 0.9956

_diffrn_measured_fraction_theta_max 0.9956

_diffrn_measurement_details

;

#__ type_ start__ end____ width___ exp.time_

1 omega 150.00 178.00 1.0000 2.9900

omega____ theta____ kappa____ phi______ frames

- 108.0000 43.0000 30.0000 28


2 omega 131.00 156.00 1.0000 2.9900


- 108.0000 54.0000 60.0000 25


3 omega 118.00 146.00 1.0000 2.9900


- 66.4657 64.0000 150.0000 28


4 omega 107.00 132.00 1.0000 2.9900


- 66.4657 111.0000 150.0000 25


5 omega 101.00 176.00 1.0000 2.9900


- 108.0000 104.0000 60.0000 75


6 omega 152.00 178.00 1.0000 2.9900


- 108.0000 138.0000 -30.0000 26


7 omega 138.00 175.00 1.0000 2.9900


- 108.0000 104.0000 -120.0000 37


8 omega 142.00 176.00 1.0000 2.9900


- 108.0000 104.0000 -150.0000 34


9 omega 130.00 176.00 1.0000 2.9900


- 108.0000 104.0000 -60.0000 46


10 omega 125.00 151.00 1.0000 2.9900


- 66.4657 111.0000 -180.0000 26


11 omega 109.00 135.00 1.0000 2.9900


- 108.0000 54.0000 -90.0000 26


12 omega 66.00 91.00 1.0000 2.9900


- 108.0000 -32.0000 -180.0000 25


13 omega 66.00 91.00 1.0000 2.9900


- 108.0000 -21.0000 -180.0000 25


14 omega 61.00 109.00 1.0000 2.9900


- 108.0000 -54.0000 -120.0000 48


15 omega 110.00 150.00 1.0000 2.9900


- 108.0000 -77.0000 -60.0000 40


16 omega 71.00 97.00 1.0000 2.9900


- 108.0000 -43.0000 90.0000 26


17 omega 54.00 79.00 1.0000 2.9900


- 108.0000 -21.0000 120.0000 25


18 omega 46.00 78.00 1.0000 2.9900


- 108.0000 -54.0000 90.0000 32


19 omega 49.00 178.00 1.0000 2.9900


- 108.0000 -11.0000 60.0000 129


20 omega 86.00 111.00 1.0000 2.9900


- 108.0000 54.0000 60.0000 25


21 omega 57.00 146.00 1.0000 2.9900


- 66.4657 50.0000 -30.0000 89


22 omega 65.00 91.00 1.0000 2.9900


- 108.0000 -21.0000 -90.0000 26


23 omega 47.00 90.00 1.0000 2.9900


- 66.4657 -38.0000 -180.0000 43


24 omega 29.00 107.00 1.0000 2.9900


- 108.0000 -54.0000 -180.0000 78


25 omega 68.00 112.00 1.0000 2.9900


- 108.0000 43.0000 30.0000 44


26 omega 33.00 88.00 1.0000 2.9900


- 66.4657 64.0000 150.0000 55


27 omega 34.00 59.00 1.0000 1.0000


- -24.9315 38.0000 120.0000 25


28 omega -9.00 61.00 1.0000 2.9900


- 66.4657 -50.0000 30.0000 70


29 omega 35.00 84.00 1.0000 2.9900


- 108.0000 -104.0000 90.0000 49


30 omega 49.00 111.00 1.0000 2.9900


- 108.0000 -104.0000 120.0000 62


31 omega 23.00 108.00 1.0000 2.9900


- 108.0000 -112.0000 63.0000 85


32 omega -7.00 19.00 1.0000 2.9900


- 66.4657 -38.0000 -180.0000 26


33 omega -48.00 42.00 1.0000 1.0000


- -24.9315 38.0000 30.0000 90


34 omega -49.00 -11.00 1.0000 1.0000


- -24.9315 38.0000 120.0000 38


35 omega -115.00 -34.00 1.0000 1.0000


- -24.9315 178.0000 60.0000 81


36 omega 66.00 151.00 1.0000 2.9900


- 66.4657 178.0000 -90.0000 85


37 omega -93.00 -47.00 1.0000 1.0000


- -24.9315 -178.0000 -180.0000 46

;

_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 0.0838230000

_diffrn_orient_matrix_UB_12 -0.0255813000








_diffrn_radiation_monochromator mirror

_diffrn_radiation_probe x-ray

_diffrn_radiation_type 'Cu K\a'

_diffrn_radiation_wavelength 1.54184

_diffrn_source 'sealed X-ray tube'

_diffrn_source_type 'SuperNova (Cu) X-ray Source'

_diffrn_standards_decay_% ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time ?

_diffrn_standards_number ?

_reflns_number_gt 5495

_reflns_number_total 6289

_reflns_odcompleteness_completeness 95.80

_reflns_odcompleteness_iscentric 1

_reflns_odcompleteness_theta 66.97

_reflns_threshold_expression >2sigma(I)

_computing_cell_refinement

;



(compiled Apr 11 2014,15:12:41)

;

_computing_data_collection

;



(compiled Apr 11 2014,15:12:41)

;

_computing_data_reduction

;



(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 0.742

_refine_diff_density_min -0.726

_refine_diff_density_rms 0.078

_refine_ls_extinction_coef ?

_refine_ls_extinction_method none

_refine_ls_goodness_of_fit_ref 1.053

_refine_ls_hydrogen_treatment mixed

_refine_ls_matrix_type full

_refine_ls_number_parameters 531

_refine_ls_number_reflns 6289

_refine_ls_number_restraints 0

_refine_ls_R_factor_all 0.0642

_refine_ls_R_factor_gt 0.0581

_refine_ls_restrained_S_all 1.053

_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^)+(0.0961P)^2^+2.4851P] where P=(Fo^2^+2Fc^2^)/3'

_refine_ls_weighting_scheme calc

_refine_ls_wR_factor_gt 0.1591

_refine_ls_wR_factor_ref 0.1675

_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.

;

_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

Cl2 Cl 0.85937(9) 0.11336(5) -0.00741(5) 0.0511(2) Uani 1 1 d . . .

Cl1 Cl 0.61272(10) 0.05494(9) -0.05657(7) 0.0838(4) Uani 1 1 d . . .

C39 C 0.7720(4) 0.0401(2) -0.0318(3) 0.0613(11) Uani 1 1 d . . .

H39A H 0.8076 0.0182 -0.0744 0.074 Uiso 1 1 calc R . .

H39B H 0.7804 0.0091 0.0112 0.074 Uiso 1 1 calc R . .

F10 F 0.88861(13) 0.20393(8) 0.30359(9) 0.0266(3) Uani 1 1 d . . .

F8 F 1.14575(14) 0.09877(9) 0.13640(10) 0.0333(4) Uani 1 1 d . . .

F6 F 0.76434(14) -0.00208(8) 0.18174(9) 0.0293(4) Uani 1 1 d . . .

F1 F 0.40880(13) 0.09628(8) 0.25262(9) 0.0269(4) Uani 1 1 d . . .

F11 F 0.53561(13) 0.07527(8) 0.42754(9) 0.0279(4) Uani 1 1 d . . .

F9 F 1.09712(14) 0.20369(9) 0.23008(9) 0.0301(4) Uani 1 1 d . . .

F2 F 0.27470(14) -0.01516(9) 0.22804(10) 0.0323(4) Uani 1 1 d . . .

F7 F 0.97552(15) -0.00424(9) 0.11639(10) 0.0347(4) Uani 1 1 d . . .

F3 F 0.38341(15) -0.13891(9) 0.25822(11) 0.0383(4) Uani 1 1 d . . .

F5 F 0.76937(13) -0.03512(8) 0.33220(9) 0.0277(4) Uani 1 1 d . . .

F14 F 1.02597(15) 0.08102(11) 0.53452(11) 0.0432(5) Uani 1 1 d . . .

F12 F 0.59673(16) 0.05780(9) 0.57402(10) 0.0362(4) Uani 1 1 d . . .

F15 F 0.96887(13) 0.09877(10) 0.38915(10) 0.0344(4) Uani 1 1 d . . .

F4 F 0.62846(15) -0.14608(8) 0.31422(11) 0.0345(4) Uani 1 1 d . . .

F13 F 0.84415(17) 0.06140(11) 0.63259(10) 0.0420(4) Uani 1 1 d . . .

N1 N 0.56055(18) 0.22248(11) 0.31458(12) 0.0208(5) Uani 1 1 d . . .

C26 C 0.6468(2) -0.02759(15) 0.30530(16) 0.0245(6) Uani 1 1 d . . .

C34 C 0.6591(2) 0.08099(13) 0.45114(16) 0.0239(5) Uani 1 1 d . . .

C25 C 0.5765(2) -0.08563(15) 0.29549(16) 0.0265(6) Uani 1 1 d . . .

C21 C 0.5996(2) 0.03709(14) 0.28866(14) 0.0220(5) Uani 1 1 d . . .

C28 C 0.8449(2) 0.04878(14) 0.20099(16) 0.0250(5) Uani 1 1 d . . .

C32 C 0.9067(2) 0.15028(14) 0.25820(15) 0.0229(5) Uani 1 1 d . . .

C36 C 0.8125(3) 0.07114(15) 0.55774(17) 0.0312(6) Uani 1 1 d . . .

C22 C 0.4718(2) 0.03709(14) 0.26424(15) 0.0245(5) Uani 1 1 d . . .

C1 C 0.6127(2) 0.17461(13) 0.27595(15) 0.0201(5) Uani 1 1 d . . .

C5 C 0.5535(2) 0.22572(13) 0.39855(15) 0.0224(5) Uani 1 1 d . . .

C14 C 0.7660(2) 0.29252(13) 0.41910(16) 0.0243(5) Uani 1 1 d . . .

H14 H 0.7642 0.2881 0.3634 0.029 Uiso 1 1 calc R . .

C31 C 1.0157(2) 0.15173(15) 0.22078(15) 0.0259(6) Uani 1 1 d . . .

C17 C 0.7099(2) 0.22518(15) 0.15797(16) 0.0288(6) Uani 1 1 d . . .

H17A H 0.7562 0.2494 0.1987 0.043 Uiso 1 1 calc R . .

H17B H 0.6838 0.2558 0.1172 0.043 Uiso 1 1 calc R . .

H17C H 0.7627 0.1907 0.1393 0.043 Uiso 1 1 calc R . .

C30 C 1.0412(2) 0.09896(15) 0.17386(16) 0.0274(6) Uani 1 1 d . . .

C16 C 0.7557(3) 0.36808(15) 0.43922(18) 0.0307(6) Uani 1 1 d . . .

H16A H 0.6723 0.3840 0.4229 0.046 Uiso 1 1 calc R . .

H16B H 0.8167 0.3933 0.4138 0.046 Uiso 1 1 calc R . .

H16C H 0.7717 0.3739 0.4935 0.046 Uiso 1 1 calc R . .

C27 C 0.8158(2) 0.09972(14) 0.25160(15) 0.0223(5) Uani 1 1 d . . .

C33 C 0.7448(2) 0.09581(13) 0.39758(16) 0.0223(5) Uani 1 1 d . . .

C38 C 0.8688(2) 0.09240(14) 0.43080(17) 0.0259(6) Uani 1 1 d . . .

C7 C 0.6457(2) 0.25298(15) 0.52515(16) 0.0275(6) Uani 1 1 d . . .

H7 H 0.7114 0.2712 0.5573 0.033 Uiso 1 1 calc R . .

C12 C 0.2793(2) 0.10537(15) 0.40156(18) 0.0315(6) Uani 1 1 d . . .

H12A H 0.3399 0.0744 0.3840 0.047 Uiso 1 1 calc R . .

H12B H 0.1978 0.0966 0.3752 0.047 Uiso 1 1 calc R . .

H12C H 0.2751 0.0996 0.4556 0.047 Uiso 1 1 calc R . .

C37 C 0.9033(3) 0.08139(16) 0.50804(18) 0.0309(6) Uani 1 1 d . . .

C23 C 0.3979(2) -0.01982(16) 0.25248(15) 0.0267(6) Uani 1 1 d . . .

C9 C 0.4432(2) 0.20120(14) 0.50897(16) 0.0273(6) Uani 1 1 d . . .

H9 H 0.3729 0.1842 0.5305 0.033 Uiso 1 1 calc R . .

C11 C 0.3195(2) 0.17827(14) 0.38528(16) 0.0259(6) Uani 1 1 d . . .

H11 H 0.3281 0.1828 0.3304 0.031 Uiso 1 1 calc R . .

C35 C 0.6893(3) 0.07030(15) 0.52836(17) 0.0285(6) Uani 1 1 d . . .

C18 C 0.5560(3) 0.13313(15) 0.13324(16) 0.0292(6) Uani 1 1 d . . .

H18A H 0.6131 0.0962 0.1447 0.044 Uiso 1 1 calc R . .

H18B H 0.5619 0.1477 0.0815 0.044 Uiso 1 1 calc R . .

H18C H 0.4712 0.1188 0.1392 0.044 Uiso 1 1 calc R . .

C3 C 0.4825(2) 0.24299(15) 0.18767(15) 0.0266(6) Uani 1 1 d . . .

H3A H 0.4848 0.2740 0.1450 0.032 Uiso 1 1 calc R . .

H3B H 0.4017 0.2199 0.1833 0.032 Uiso 1 1 calc R . .

C29 C 0.9546(2) 0.04746(15) 0.16414(16) 0.0273(6) Uani 1 1 d . . .

C4 C 0.5019(2) 0.28088(14) 0.26331(15) 0.0244(5) Uani 1 1 d . . .

C8 C 0.5431(3) 0.22510(15) 0.55696(17) 0.0303(6) Uani 1 1 d . . .

H8 H 0.5416 0.2225 0.6098 0.036 Uiso 1 1 calc R . .

C2 C 0.5911(2) 0.19196(14) 0.18829(15) 0.0235(5) Uani 1 1 d . . .

C19 C 0.5940(2) 0.34019(15) 0.26230(16) 0.0286(6) Uani 1 1 d . . .

H19A H 0.5993 0.3628 0.3109 0.043 Uiso 1 1 calc R . .

H19B H 0.5644 0.3713 0.2227 0.043 Uiso 1 1 calc R . .

H19C H 0.6760 0.3237 0.2526 0.043 Uiso 1 1 calc R . .

C6 C 0.6531(2) 0.25453(13) 0.44593(15) 0.0232(5) Uani 1 1 d . . .

C20 C 0.3797(2) 0.30871(16) 0.28895(17) 0.0309(6) Uani 1 1 d . . .

H20A H 0.3148 0.2750 0.2818 0.046 Uiso 1 1 calc R . .

H20B H 0.3549 0.3480 0.2592 0.046 Uiso 1 1 calc R . .

H20C H 0.3921 0.3208 0.3421 0.046 Uiso 1 1 calc R . .

C15 C 0.8938(2) 0.26667(15) 0.45528(16) 0.0284(6) Uani 1 1 d . . .

H15A H 0.9608 0.2912 0.4345 0.043 Uiso 1 1 calc R . .

H15B H 0.9019 0.2194 0.4443 0.043 Uiso 1 1 calc R . .

H15C H 0.8988 0.2732 0.5097 0.043 Uiso 1 1 calc R . .

C24 C 0.4514(2) -0.08226(15) 0.26765(17) 0.0279(6) Uani 1 1 d . . .

B1 B 0.6932(2) 0.10341(15) 0.30495(17) 0.0214(6) Uani 1 1 d . . .

C10 C 0.4429(2) 0.20146(13) 0.42952(16) 0.0241(5) Uani 1 1 d . . .

C13 C 0.2111(2) 0.22472(16) 0.40652(18) 0.0314(6) Uani 1 1 d . . .

H13A H 0.1362 0.2152 0.3735 0.047 Uiso 1 1 calc R . .

H13B H 0.2349 0.2711 0.4006 0.047 Uiso 1 1 calc R . .

H13C H 0.1949 0.2167 0.4587 0.047 Uiso 1 1 calc R . .

loop_

_atom_site_aniso_label

_atom_site_aniso_U_11






Cl2 0.0744(6) 0.0397(5) 0.0393(4) 0.0034(4) 0.0055(4) 0.0005(4)

Cl1 0.0526(6) 0.1292(12) 0.0703(7) -0.0396(8) 0.0097(5) 0.0111(6)

C39 0.061(2) 0.048(2) 0.071(3) -0.008(2) -0.009(2) 0.0013(19)

F10 0.0232(7) 0.0254(8) 0.0316(8) -0.0057(7) 0.0042(6) -0.0023(6)

F8 0.0229(7) 0.0392(10) 0.0395(9) 0.0011(8) 0.0130(7) 0.0007(7)

F6 0.0259(8) 0.0280(8) 0.0348(8) -0.0073(7) 0.0076(6) -0.0052(6)

F1 0.0177(7) 0.0279(8) 0.0344(8) -0.0006(7) -0.0018(6) 0.0017(6)

F11 0.0164(7) 0.0343(9) 0.0331(8) -0.0008(7) 0.0029(6) -0.0006(6)

F9 0.0224(7) 0.0328(9) 0.0352(9) 0.0000(7) 0.0034(6) -0.0079(6)

F2 0.0174(7) 0.0361(9) 0.0425(9) -0.0023(8) -0.0021(6) -0.0040(6)

F7 0.0337(9) 0.0312(9) 0.0412(10) -0.0080(8) 0.0147(7) -0.0004(7)

F3 0.0268(8) 0.0306(9) 0.0571(11) -0.0036(8) 0.0024(7) -0.0103(7)

F5 0.0170(7) 0.0270(8) 0.0386(9) 0.0009(7) -0.0005(6) 0.0042(6)

F14 0.0227(8) 0.0635(13) 0.0409(10) 0.0091(9) -0.0109(7) -0.0013(8)

F12 0.0343(9) 0.0439(10) 0.0319(9) 0.0045(8) 0.0117(7) 0.0006(7)

F15 0.0140(7) 0.0538(11) 0.0353(9) 0.0082(8) 0.0012(6) -0.0007(7)

F4 0.0278(8) 0.0227(8) 0.0536(11) 0.0030(8) 0.0077(7) 0.0009(6)

F13 0.0450(10) 0.0519(12) 0.0277(9) 0.0065(8) -0.0046(7) -0.0021(8)

N1 0.0135(9) 0.0220(11) 0.0268(11) 0.0009(9) 0.0006(8) -0.0007(8)

C26 0.0153(11) 0.0292(14) 0.0292(13) -0.0002(11) 0.0039(9) -0.0005(10)

C34 0.0174(12) 0.0229(13) 0.0310(14) -0.0004(11) 0.0006(10) 0.0010(10)

C25 0.0224(12) 0.0252(14) 0.0327(14) 0.0015(12) 0.0072(10) 0.0021(11)

C21 0.0177(11) 0.0255(13) 0.0230(12) -0.0008(11) 0.0032(9) -0.0018(10)

C28 0.0214(12) 0.0227(13) 0.0306(14) 0.0017(11) 0.0013(10) 0.0000(10)

C32 0.0203(12) 0.0243(13) 0.0238(12) -0.0009(11) -0.0003(9) 0.0037(10)

C36 0.0344(15) 0.0318(15) 0.0262(14) 0.0020(12) -0.0035(11) 0.0016(12)

C22 0.0201(12) 0.0252(13) 0.0281(13) -0.0010(11) 0.0023(10) 0.0026(10)

C1 0.0111(10) 0.0227(13) 0.0264(13) -0.0014(11) 0.0008(9) -0.0039(9)

C5 0.0179(11) 0.0224(13) 0.0266(13) -0.0014(11) 0.0011(9) 0.0028(10)

C14 0.0192(12) 0.0238(13) 0.0296(13) -0.0036(11) 0.0002(10) -0.0015(10)

C31 0.0185(12) 0.0297(15) 0.0289(14) 0.0048(12) -0.0011(10) -0.0030(10)

C17 0.0252(13) 0.0324(15) 0.0295(14) 0.0035(12) 0.0066(10) 0.0025(11)

C30 0.0191(12) 0.0337(15) 0.0301(14) 0.0040(12) 0.0063(10) 0.0042(11)

C16 0.0274(13) 0.0254(14) 0.0386(16) -0.0030(12) -0.0005(11) -0.0018(11)

C27 0.0161(11) 0.0265(13) 0.0242(12) 0.0036(11) 0.0005(9) 0.0030(10)

C33 0.0172(11) 0.0194(12) 0.0300(14) -0.0016(11) 0.0008(10) 0.0005(9)

C38 0.0154(11) 0.0286(14) 0.0338(14) 0.0014(12) 0.0026(10) -0.0018(10)

C7 0.0232(12) 0.0304(14) 0.0279(14) -0.0045(12) -0.0028(10) 0.0009(11)

C12 0.0183(12) 0.0342(16) 0.0423(16) 0.0003(13) 0.0050(11) -0.0061(11)

C37 0.0210(13) 0.0350(15) 0.0352(15) 0.0039(13) -0.0060(11) -0.0005(11)

C23 0.0154(12) 0.0376(16) 0.0271(13) -0.0040(12) 0.0014(9) -0.0029(11)

C9 0.0233(12) 0.0280(14) 0.0312(14) -0.0001(12) 0.0056(10) -0.0004(11)

C11 0.0161(12) 0.0297(15) 0.0320(14) -0.0027(12) 0.0027(10) -0.0019(10)

C35 0.0279(13) 0.0273(14) 0.0312(14) 0.0015(12) 0.0068(11) 0.0005(11)

C18 0.0302(14) 0.0313(15) 0.0254(13) -0.0013(12) -0.0015(10) 0.0026(11)

C3 0.0207(12) 0.0311(14) 0.0272(13) -0.0003(12) -0.0018(10) 0.0020(11)

C29 0.0261(13) 0.0269(14) 0.0294(14) -0.0021(12) 0.0042(10) 0.0039(11)

C4 0.0202(12) 0.0254(13) 0.0274(13) 0.0033(11) -0.0001(9) 0.0037(10)

C8 0.0280(13) 0.0355(16) 0.0278(14) -0.0017(12) 0.0047(11) 0.0009(12)

C2 0.0199(12) 0.0265(13) 0.0240(13) 0.0029(11) 0.0008(9) -0.0001(10)

C19 0.0253(13) 0.0272(14) 0.0325(14) 0.0015(12) -0.0012(10) 0.0003(11)

C6 0.0198(12) 0.0210(12) 0.0289(13) -0.0002(11) 0.0021(10) 0.0024(10)

C20 0.0212(13) 0.0344(15) 0.0369(15) 0.0027(13) 0.0016(11) 0.0074(11)

C15 0.0202(12) 0.0311(15) 0.0334(14) -0.0056(12) -0.0005(10) -0.0016(11)

C24 0.0223(13) 0.0275(14) 0.0345(15) -0.0035(12) 0.0051(10) -0.0070(11)

B1 0.0150(12) 0.0221(14) 0.0271(15) -0.0007(12) 0.0013(10) -0.0009(11)

C10 0.0188(12) 0.0223(13) 0.0313(14) -0.0006(11) 0.0030(10) 0.0027(10)

C13 0.0164(12) 0.0378(16) 0.0404(16) -0.0051(13) 0.0049(10) 0.0015(11)

_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

Cl2 C39 1.755(4) . ?

Cl1 C39 1.734(4) . ?

F10 C32 1.351(3) . ?

F8 C30 1.341(3) . ?

F6 C28 1.345(3) . ?

F1 C22 1.355(3) . ?

F11 C34 1.345(3) . ?

F9 C31 1.344(3) . ?

F2 C23 1.344(3) . ?

F7 C29 1.354(3) . ?

F3 C24 1.336(3) . ?

F5 C26 1.353(3) . ?

F14 C37 1.344(3) . ?

F12 C35 1.346(3) . ?

F15 C38 1.350(3) . ?

F4 C25 1.346(3) . ?

F13 C36 1.340(3) . ?

N1 C1 1.316(3) . ?

N1 C5 1.483(3) . ?

N1 C4 1.560(3) . ?

C26 C25 1.373(4) . ?

C26 C21 1.396(4) . ?

C34 C33 1.397(4) . ?

C34 C35 1.380(4) . ?

C25 C24 1.376(4) . ?

C21 C22 1.388(4) . ?

C21 B1 1.656(4) . ?

C28 C27 1.396(4) . ?

C28 C29 1.384(4) . ?

C32 C31 1.383(4) . ?

C32 C27 1.388(4) . ?

C36 C37 1.373(4) . ?

C36 C35 1.364(4) . ?

C22 C23 1.378(4) . ?

C1 C2 1.573(3) . ?

C1 B1 1.702(4) . ?

C5 C6 1.406(4) . ?

C5 C10 1.423(4) . ?

C14 C16 1.543(4) . ?

C14 C6 1.526(4) . ?

C14 C15 1.535(3) . ?

C31 C30 1.372(4) . ?

C17 C2 1.559(4) . ?

C30 C29 1.374(4) . ?

C27 B1 1.674(4) . ?

C33 C38 1.394(4) . ?

C33 B1 1.675(4) . ?

C38 C37 1.389(4) . ?

C7 C8 1.383(4) . ?

C7 C6 1.400(4) . ?

C12 C11 1.539(4) . ?

C23 C24 1.376(4) . ?

C9 C8 1.378(4) . ?

C9 C10 1.394(4) . ?

C11 C10 1.532(3) . ?

C11 C13 1.546(4) . ?

C18 C2 1.537(4) . ?

C3 C4 1.522(4) . ?

C3 C2 1.533(4) . ?

C4 C19 1.530(4) . ?

C4 C20 1.515(4) . ?

loop_

_geom_angle_atom_site_label_1



_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag

Cl1 C39 Cl2 113.8(2) . . ?

C1 N1 C5 127.1(2) . . ?

C1 N1 C4 113.7(2) . . ?

C5 N1 C4 119.2(2) . . ?

F5 C26 C25 116.6(2) . . ?

F5 C26 C21 119.4(2) . . ?

C25 C26 C21 124.0(2) . . ?

F11 C34 C33 119.2(2) . . ?

F11 C34 C35 115.0(2) . . ?

C35 C34 C33 125.8(2) . . ?

F4 C25 C26 120.4(2) . . ?

F4 C25 C24 119.5(3) . . ?

C26 C25 C24 120.1(3) . . ?

C26 C21 B1 119.5(2) . . ?

C22 C21 C26 112.8(2) . . ?

C22 C21 B1 127.5(2) . . ?

F6 C28 C27 121.9(2) . . ?

F6 C28 C29 114.4(2) . . ?

C29 C28 C27 123.7(2) . . ?

F10 C32 C31 115.7(2) . . ?

F10 C32 C27 118.8(2) . . ?

C31 C32 C27 125.6(3) . . ?

F13 C36 C37 121.0(3) . . ?

F13 C36 C35 121.1(3) . . ?

C35 C36 C37 117.9(3) . . ?

F1 C22 C21 120.2(2) . . ?

F1 C22 C23 114.7(2) . . ?

C23 C22 C21 125.1(3) . . ?

N1 C1 C2 108.4(2) . . ?

N1 C1 B1 131.7(2) . . ?

C2 C1 B1 119.9(2) . . ?

C6 C5 N1 120.1(2) . . ?

C6 C5 C10 121.0(2) . . ?

C10 C5 N1 118.8(2) . . ?

C6 C14 C16 109.5(2) . . ?

C6 C14 C15 113.5(2) . . ?

C15 C14 C16 107.9(2) . . ?

F9 C31 C32 121.1(2) . . ?

F9 C31 C30 119.7(2) . . ?

C30 C31 C32 119.2(2) . . ?

F8 C30 C31 120.9(2) . . ?

F8 C30 C29 120.8(3) . . ?

C31 C30 C29 118.2(2) . . ?

C28 C27 B1 128.0(2) . . ?

C32 C27 C28 112.5(2) . . ?

C32 C27 B1 119.5(2) . . ?

C34 C33 B1 119.7(2) . . ?

C38 C33 C34 110.9(2) . . ?

C38 C33 B1 128.6(2) . . ?

F15 C38 C33 122.1(2) . . ?

F15 C38 C37 113.1(2) . . ?

C37 C38 C33 124.9(3) . . ?

C8 C7 C6 121.8(2) . . ?

F14 C37 C36 119.7(3) . . ?

F14 C37 C38 120.0(3) . . ?

C36 C37 C38 120.3(2) . . ?

F2 C23 C22 121.1(3) . . ?

F2 C23 C24 119.8(3) . . ?

C24 C23 C22 119.1(2) . . ?

C8 C9 C10 122.8(3) . . ?

C12 C11 C13 106.7(2) . . ?

C10 C11 C12 115.2(2) . . ?

C10 C11 C13 108.8(2) . . ?

F12 C35 C34 119.7(2) . . ?

F12 C35 C36 120.4(3) . . ?

C36 C35 C34 120.0(3) . . ?

C4 C3 C2 106.0(2) . . ?

F7 C29 C28 119.7(2) . . ?

F7 C29 C30 119.5(2) . . ?

C30 C29 C28 120.8(3) . . ?

C3 C4 N1 98.8(2) . . ?

C3 C4 C19 113.8(2) . . ?

C19 C4 N1 110.6(2) . . ?

C20 C4 N1 114.0(2) . . ?

C20 C4 C3 112.7(2) . . ?

C20 C4 C19 106.9(2) . . ?

C9 C8 C7 118.8(3) . . ?

C17 C2 C1 112.0(2) . . ?

C18 C2 C1 117.1(2) . . ?

C18 C2 C17 105.3(2) . . ?

C3 C2 C1 101.2(2) . . ?

C3 C2 C17 110.6(2) . . ?

C3 C2 C18 110.8(2) . . ?

C5 C6 C14 126.0(2) . . ?

C7 C6 C5 118.1(2) . . ?

C7 C6 C14 115.7(2) . . ?

F3 C24 C25 119.8(3) . . ?

F3 C24 C23 121.4(2) . . ?

C25 C24 C23 118.8(3) . . ?

C21 B1 C1 109.11(19) . . ?

C21 B1 C27 110.8(2) . . ?

C21 B1 C33 103.6(2) . . ?

C27 B1 C1 105.3(2) . . ?

C27 B1 C33 109.63(19) . . ?

C33 B1 C1 118.4(2) . . ?

C5 C10 C11 127.3(2) . . ?

C9 C10 C5 117.1(2) . . ?

C9 C10 C11 115.5(2) . . ?

_olex2_refinement_description

;

1. Fixed Uiso

At 1.2 times of:

H14 of C14, H11 of C11, H7 of C7, H9 of C9, {H3a,H3b} of C3, {H39a,H39b} of

C39, H8 of C8

At 1.5 times of:

{H17a,H17b,H17c} of C17, {H16a,H16b,H16c} of C16, {H12a,H12b,H12c} of C12,

{H18a,H18b,H18c} of C18, {H13a,H13b,H13c} of C13, {H19a,H19b,H19c} of C19,

{H15a,H15b,H15c} of C15, {H20a,H20b,H20c} of C20

2.a Ternary CH refined with riding coordinates:

C14(H14), C11(H11)

2.b Secondary CH2 refined with riding coordinates:

C39(H39a,H39b), C3(H3a,H3b)

2.c Aromatic/amide H refined with riding coordinates:

C7(H7), C9(H9), C8(H8)

2.d Idealised Me refined as rotating group:

C17(H17a,H17b,H17c), C16(H16a,H16b,H16c), C12(H12a,H12b,H12c), C18(H18a,H18b,

H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C15(H15a,H15b,H15c), C13(H13a,

H13b,H13c)

;

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