data_1
_audit_creation_date 2015-01-21
_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 GBBC6F5
_chemical_formula_moiety 'C57 H44 B F15 N2'
_chemical_formula_sum 'C57 H44 B F15 N2'
_chemical_formula_weight 1052.75
_chemical_melting_point ?
_chemical_oxdiff_formula 'C21 H18 N2 B F15'
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'
_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 12.2212(5)
_cell_length_b 23.0961(9)
_cell_length_c 19.3645(7)
_cell_angle_alpha 90.00
_cell_angle_beta 99.943(4)
_cell_angle_gamma 90.00
_cell_volume 5383.8(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 6998
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 24.9810
_cell_measurement_theta_min 2.0330
_exptl_absorpt_coefficient_mu 0.112
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.79005
_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 whitish colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier whitish
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.299
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2160
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.39
_exptl_crystal_size_min 0.21
_exptl_special_details
;
?
;
_diffrn_reflns_av_R_equivalents 0.0328
_diffrn_reflns_av_unetI/netI 0.0533
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 17857
_diffrn_reflns_theta_full 25.03
_diffrn_reflns_theta_max 25.03
_diffrn_reflns_theta_min 1.76
_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 0.9991
_diffrn_measured_fraction_theta_max 0.9991
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega 43.00 115.00 1.0000 32.6200
omega____ theta____ kappa____ phi______frames
- 27.5074 178.0000 150.0000 72
#__ type_ start__ end____ width___ exp.time_
2 omega 56.00 95.00 1.0000 32.6200
omega____ theta____ kappa____ phi______frames
- 27.5074 178.0000 30.0000 39
#__ type_ start__ end____ width___ exp.time_
3 omega 12.00 53.00 1.0000 32.6200
omega____ theta____ kappa____ phi______frames
- 27.5074 57.0000 150.0000 41
#__ type_ start__ end____ width___ exp.time_
4 omega -10.00 89.00 1.0000 32.6200
omega____ theta____ kappa____ phi______frames
- 27.5074 77.0000 -150.0000 99
;
_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 -0.0462757000
_diffrn_orient_matrix_UB_12 -0.0184239000
_diffrn_orient_matrix_UB_13 0.0007458000
_diffrn_orient_matrix_UB_21 -0.0212694000
_diffrn_orient_matrix_UB_22 0.0199182000
_diffrn_orient_matrix_UB_23 0.0222082000
_diffrn_orient_matrix_UB_31 -0.0297102000
_diffrn_orient_matrix_UB_32 0.0143557000
_diffrn_orient_matrix_UB_33 -0.0298113000
_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 7274
_reflns_number_total 9487
_reflns_odcompleteness_completeness 86.43
_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
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_refine_diff_density_max 0.242
_refine_diff_density_min -0.236
_refine_diff_density_rms 0.054
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.041
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 684
_refine_ls_number_reflns 9487
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0593
_refine_ls_R_factor_gt 0.0462
_refine_ls_restrained_S_all 1.041
_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^)+(0.0579P)^2^+0.6397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1165
_refine_ls_wR_factor_ref 0.1233
_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:
H25 of C25, H24 of C24, H34 of C34, H37 of C37, H26 of C26, H9 of C9, H8 of
C8, H7 of C7, H5 of C5, H21 of C21, H6 of C6, H20 of C20, H19 of C19, H18 of
C18, H12 of C12, H13 of C13, H28 of C28, H14 of C14, H31 of C31, H17 of C17
At 1.5 times of:
{H38A,H38B,H38C} of C38, {H36A,H36B,H36C} of C36, {H32A,H32B,H32C} of C32,
{H33A,H33B,H33C} of C33, {H35A,H35B,H35C} of C35, {H39A,H39B,H39C} of C39,
{H30A,H30B,H30C} of C30, {H29A,H29B,H29C} of C29
2.a Ternary CH refined with riding coordinates:
C28(H28), C31(H31), C34(H34), C37(H37)
2.b Aromatic/amide H refined with riding coordinates:
C14(H14), C13(H13), C12(H12), C26(H26), C25(H25), C24(H24), C9(H9), C8(H8),
C7(H7), C6(H6), C5(H5), C21(H21), C20(H20), C19(H19), C18(H18), C17(H17)
2.c Idealised Me refined as rotating group:
C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C32(H32A,H32B,
H32C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,
H39B,H39C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary iterative
_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
F11 F 0.79338(10) 0.01411(5) 0.21613(6) 0.0332(3) Uani 1 1 d . . .
F12 F 0.89015(12) -0.02640(6) 0.11636(8) 0.0481(4) Uani 1 1 d . . .
F15 F 1.03092(9) 0.17860(5) 0.23172(6) 0.0244(3) Uani 1 1 d . . .
F13 F 1.05250(12) 0.03422(6) 0.06721(7) 0.0474(4) Uani 1 1 d . . .
F14 F 1.11937(10) 0.13768(6) 0.12810(6) 0.0358(3) Uani 1 1 d . . .
F6 F 0.93447(9) 0.24110(5) 0.38024(6) 0.0274(3) Uani 1 1 d . . .
F7 F 1.13620(11) 0.26630(6) 0.44359(7) 0.0422(3) Uani 1 1 d . . .
F10 F 1.05369(9) 0.05029(5) 0.33959(6) 0.0306(3) Uani 1 1 d . . .
F8 F 1.30426(10) 0.18648(7) 0.45297(7) 0.0453(4) Uani 1 1 d . . .
F9 F 1.25965(10) 0.07930(6) 0.40013(7) 0.0383(3) Uani 1 1 d . . .
F5 F 0.93611(10) 0.06014(6) 0.44439(6) 0.0340(3) Uani 1 1 d . . .
F4 F 0.82087(12) -0.01478(6) 0.50030(7) 0.0485(4) Uani 1 1 d . . .
F1 F 0.63517(9) 0.08226(5) 0.25383(6) 0.0297(3) Uani 1 1 d . . .
F3 F 0.60813(12) -0.04305(6) 0.43885(7) 0.0479(4) Uani 1 1 d . . .
F2 F 0.51894(10) 0.00823(6) 0.31473(7) 0.0408(3) Uani 1 1 d . . .
N1 N 0.75344(12) 0.22249(7) 0.23671(8) 0.0172(3) Uani 1 1 d . . .
N2 N 0.64419(13) 0.24699(7) 0.30932(8) 0.0173(3) Uani 1 1 d . . .
C40 C 0.79630(16) 0.07473(9) 0.34227(10) 0.0229(4) Uani 1 1 d . . .
C45 C 0.83507(17) 0.04753(9) 0.40617(11) 0.0264(5) Uani 1 1 d . . .
C44 C 0.77542(19) 0.00798(10) 0.43796(11) 0.0327(5) Uani 1 1 d . . .
C43 C 0.66918(19) -0.00613(10) 0.40763(12) 0.0325(5) Uani 1 1 d . . .
C42 C 0.62485(17) 0.01982(9) 0.34483(12) 0.0279(5) Uani 1 1 d . . .
C41 C 0.68771(17) 0.05814(9) 0.31454(11) 0.0250(5) Uani 1 1 d . . .
C46 C 0.98086(16) 0.14404(9) 0.35460(10) 0.0221(4) Uani 1 1 d . . .
C47 C 1.01041(16) 0.19783(9) 0.38429(10) 0.0244(5) Uani 1 1 d . . .
C48 C 1.11559(17) 0.21255(10) 0.41788(10) 0.0290(5) Uani 1 1 d . . .
C49 C 1.20031(17) 0.17276(11) 0.42301(10) 0.0307(5) Uani 1 1 d . . .
C50 C 1.17707(17) 0.11852(10) 0.39579(11) 0.0293(5) Uani 1 1 d . . .
C51 C 1.07035(17) 0.10539(9) 0.36358(10) 0.0246(5) Uani 1 1 d . . .
C2 C 0.77285(15) 0.18118(8) 0.29153(9) 0.0178(4) Uani 1 1 d . . .
C1 C 0.67662(15) 0.26206(8) 0.24862(9) 0.0177(4) Uani 1 1 d . . .
C3 C 0.70240(16) 0.19724(8) 0.33601(10) 0.0191(4) Uani 1 1 d . . .
C52 C 0.90443(16) 0.10003(8) 0.23165(10) 0.0212(4) Uani 1 1 d . . .
C53 C 0.87494(16) 0.04754(9) 0.19869(11) 0.0250(5) Uani 1 1 d . . .
C54 C 0.92448(19) 0.02495(9) 0.14505(12) 0.0320(5) Uani 1 1 d . . .
C55 C 1.00616(18) 0.05497(10) 0.12051(11) 0.0320(5) Uani 1 1 d . . .
C56 C 1.03894(17) 0.10713(9) 0.15077(10) 0.0258(5) Uani 1 1 d . . .
C57 C 0.98917(16) 0.12753(9) 0.20494(10) 0.0216(4) Uani 1 1 d . . .
C10 C 0.56572(16) 0.27893(8) 0.34335(10) 0.0197(4) Uani 1 1 d . . .
C15 C 0.45258(16) 0.27592(9) 0.31562(10) 0.0226(4) Uani 1 1 d . . .
C14 C 0.38187(17) 0.31175(10) 0.34568(10) 0.0269(5) Uani 1 1 d . . .
H14 H 0.3060 0.3110 0.3285 0.032 Uiso 1 1 calc R . .
C13 C 0.42282(18) 0.34832(10) 0.40056(11) 0.0294(5) Uani 1 1 d . . .
H13 H 0.3748 0.3730 0.4187 0.035 Uiso 1 1 calc R . .
C12 C 0.53505(17) 0.34843(9) 0.42876(10) 0.0263(5) Uani 1 1 d . . .
H12 H 0.5609 0.3722 0.4669 0.032 Uiso 1 1 calc R . .
C11 C 0.60953(16) 0.31380(9) 0.40115(10) 0.0217(4) Uani 1 1 d . . .
C28 C 0.73269(17) 0.31499(9) 0.43222(10) 0.0250(5) Uani 1 1 d . . .
H28 H 0.7669 0.2813 0.4138 0.030 Uiso 1 1 calc R . .
C29 C 0.79202(19) 0.36864(11) 0.41142(12) 0.0381(6) Uani 1 1 d . . .
H29A H 0.7820 0.3712 0.3612 0.057 Uiso 1 1 calc R . .
H29B H 0.8699 0.3660 0.4302 0.057 Uiso 1 1 calc R . .
H29C H 0.7616 0.4025 0.4297 0.057 Uiso 1 1 calc R . .
C30 C 0.75171(19) 0.30904(12) 0.51234(11) 0.0379(6) Uani 1 1 d . . .
H30A H 0.7288 0.3440 0.5326 0.057 Uiso 1 1 calc R . .
H30B H 0.8292 0.3024 0.5295 0.057 Uiso 1 1 calc R . .
H30C H 0.7091 0.2770 0.5250 0.057 Uiso 1 1 calc R . .
C31 C 0.40437(17) 0.23701(10) 0.25415(10) 0.0275(5) Uani 1 1 d . . .
H31 H 0.4652 0.2140 0.2414 0.033 Uiso 1 1 calc R . .
C33 C 0.31712(18) 0.19529(11) 0.27304(12) 0.0358(6) Uani 1 1 d . . .
H33A H 0.3478 0.1742 0.3146 0.054 Uiso 1 1 calc R . .
H33B H 0.2953 0.1687 0.2351 0.054 Uiso 1 1 calc R . .
H33C H 0.2534 0.2168 0.2813 0.054 Uiso 1 1 calc R . .
C32 C 0.35305(19) 0.27260(11) 0.19001(11) 0.0346(5) Uani 1 1 d . . .
H32A H 0.2912 0.2944 0.2008 0.052 Uiso 1 1 calc R . .
H32B H 0.3280 0.2471 0.1514 0.052 Uiso 1 1 calc R . .
H32C H 0.4078 0.2986 0.1777 0.052 Uiso 1 1 calc R . .
C22 C 0.81047(16) 0.22793(8) 0.17668(10) 0.0196(4) Uani 1 1 d . . .
C27 C 0.77882(16) 0.19103(9) 0.11871(10) 0.0225(4) Uani 1 1 d . . .
C26 C 0.83558(17) 0.19850(10) 0.06263(10) 0.0270(5) Uani 1 1 d . . .
H26 H 0.8178 0.1749 0.0234 0.032 Uiso 1 1 calc R . .
C25 C 0.91765(17) 0.24010(10) 0.06390(11) 0.0303(5) Uani 1 1 d . . .
H25 H 0.9556 0.2432 0.0264 0.036 Uiso 1 1 calc R . .
C24 C 0.94327(17) 0.27667(10) 0.12013(11) 0.0272(5) Uani 1 1 d . . .
H24 H 0.9971 0.3050 0.1197 0.033 Uiso 1 1 calc R . .
C23 C 0.88974(16) 0.27203(9) 0.17824(10) 0.0232(4) Uani 1 1 d . . .
C34 C 0.92070(17) 0.31516(9) 0.23791(11) 0.0253(5) Uani 1 1 d . . .
H34 H 0.8773 0.3060 0.2746 0.030 Uiso 1 1 calc R . .
C35 C 0.89211(19) 0.37708(9) 0.21220(12) 0.0341(5) Uani 1 1 d . . .
H35A H 0.9391 0.3881 0.1795 0.051 Uiso 1 1 calc R . .
H35B H 0.9036 0.4031 0.2514 0.051 Uiso 1 1 calc R . .
H35C H 0.8158 0.3787 0.1896 0.051 Uiso 1 1 calc R . .
C36 C 1.04432(18) 0.31217(10) 0.27009(12) 0.0319(5) Uani 1 1 d . . .
H36A H 1.0629 0.2734 0.2858 0.048 Uiso 1 1 calc R . .
H36B H 1.0594 0.3383 0.3092 0.048 Uiso 1 1 calc R . .
H36C H 1.0881 0.3230 0.2355 0.048 Uiso 1 1 calc R . .
C37 C 0.68839(17) 0.14495(9) 0.11612(10) 0.0256(5) Uani 1 1 d . . .
H37 H 0.7025 0.1243 0.1610 0.031 Uiso 1 1 calc R . .
C38 C 0.6912(2) 0.10000(10) 0.05843(12) 0.0371(6) Uani 1 1 d . . .
H38A H 0.6666 0.1175 0.0135 0.056 Uiso 1 1 calc R . .
H38B H 0.6432 0.0683 0.0647 0.056 Uiso 1 1 calc R . .
H38C H 0.7658 0.0860 0.0609 0.056 Uiso 1 1 calc R . .
C39 C 0.56987(17) 0.16893(10) 0.10725(11) 0.0300(5) Uani 1 1 d . . .
H39A H 0.5626 0.1927 0.1468 0.045 Uiso 1 1 calc R . .
H39B H 0.5181 0.1374 0.1042 0.045 Uiso 1 1 calc R . .
H39C H 0.5547 0.1917 0.0652 0.045 Uiso 1 1 calc R . .
C4 C 0.68123(16) 0.17254(9) 0.40323(10) 0.0214(4) Uani 1 1 d . . .
C9 C 0.57460(17) 0.15305(9) 0.40906(11) 0.0272(5) Uani 1 1 d . . .
H9 H 0.5174 0.1561 0.3707 0.033 Uiso 1 1 calc R . .
C8 C 0.55303(18) 0.12927(10) 0.47111(11) 0.0337(5) Uani 1 1 d . . .
H8 H 0.4818 0.1166 0.4742 0.040 Uiso 1 1 calc R . .
C7 C 0.63718(19) 0.12436(10) 0.52829(11) 0.0347(6) Uani 1 1 d . . .
H7 H 0.6229 0.1081 0.5698 0.042 Uiso 1 1 calc R . .
C6 C 0.74324(19) 0.14375(10) 0.52371(11) 0.0331(5) Uani 1 1 d . . .
H6 H 0.8000 0.1407 0.5623 0.040 Uiso 1 1 calc R . .
C5 C 0.76482(18) 0.16770(9) 0.46162(10) 0.0268(5) Uani 1 1 d . . .
H5 H 0.8361 0.1807 0.4591 0.032 Uiso 1 1 calc R . .
C16 C 0.63479(15) 0.31314(8) 0.20459(10) 0.0188(4) Uani 1 1 d . . .
C21 C 0.62072(16) 0.31092(9) 0.13111(10) 0.0219(4) Uani 1 1 d . . .
H21 H 0.6407 0.2777 0.1092 0.026 Uiso 1 1 calc R . .
C20 C 0.57721(16) 0.35797(9) 0.09110(10) 0.0241(5) Uani 1 1 d . . .
H20 H 0.5685 0.3559 0.0425 0.029 Uiso 1 1 calc R . .
C19 C 0.54653(17) 0.40776(9) 0.12218(10) 0.0248(5) Uani 1 1 d . . .
H19 H 0.5160 0.4388 0.0949 0.030 Uiso 1 1 calc R . .
C18 C 0.56194(17) 0.41068(9) 0.19470(11) 0.0249(5) Uani 1 1 d . . .
H18 H 0.5425 0.4442 0.2163 0.030 Uiso 1 1 calc R . .
C17 C 0.60607(16) 0.36418(8) 0.23543(10) 0.0218(4) Uani 1 1 d . . .
H17 H 0.6167 0.3671 0.2840 0.026 Uiso 1 1 calc R . .
B1 B 0.86165(18) 0.12545(10) 0.30398(11) 0.0202(5) 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
F11 0.0349(7) 0.0253(7) 0.0399(7) -0.0040(6) 0.0079(6) -0.0061(6)
F12 0.0534(9) 0.0351(8) 0.0570(9) -0.0228(7) 0.0131(7) -0.0047(7)
F15 0.0261(6) 0.0232(6) 0.0247(6) 0.0010(5) 0.0064(5) -0.0037(5)
F13 0.0500(8) 0.0579(9) 0.0381(7) -0.0184(7) 0.0186(7) 0.0010(7)
F14 0.0341(7) 0.0458(8) 0.0312(7) 0.0021(6) 0.0157(6) -0.0015(6)
F6 0.0241(6) 0.0307(7) 0.0270(6) -0.0053(5) 0.0034(5) 0.0005(5)
F7 0.0337(7) 0.0520(9) 0.0386(7) -0.0214(7) -0.0002(6) -0.0069(7)
F10 0.0262(6) 0.0278(7) 0.0367(7) 0.0072(6) 0.0019(5) 0.0039(5)
F8 0.0218(7) 0.0719(10) 0.0381(7) -0.0137(7) -0.0061(6) -0.0033(7)
F9 0.0213(6) 0.0491(8) 0.0428(8) 0.0156(7) 0.0010(6) 0.0080(6)
F5 0.0296(7) 0.0455(8) 0.0253(6) 0.0153(6) 0.0005(5) -0.0010(6)
F4 0.0589(9) 0.0531(9) 0.0343(7) 0.0254(7) 0.0104(7) -0.0016(7)
F1 0.0242(6) 0.0276(7) 0.0350(7) 0.0052(6) -0.0008(5) -0.0009(5)
F3 0.0566(9) 0.0410(8) 0.0521(8) 0.0106(7) 0.0265(7) -0.0156(7)
F2 0.0276(7) 0.0357(7) 0.0607(9) 0.0013(7) 0.0118(6) -0.0075(6)
N1 0.0167(8) 0.0208(8) 0.0142(8) 0.0001(7) 0.0028(6) -0.0001(7)
N2 0.0174(8) 0.0214(8) 0.0131(7) 0.0001(7) 0.0025(6) 0.0008(7)
C40 0.0229(11) 0.0214(10) 0.0252(10) 0.0034(9) 0.0066(8) 0.0026(9)
C45 0.0257(11) 0.0276(11) 0.0263(11) 0.0063(9) 0.0058(9) 0.0031(9)
C44 0.0399(14) 0.0324(12) 0.0284(11) 0.0121(10) 0.0132(10) 0.0049(11)
C43 0.0388(13) 0.0251(12) 0.0393(13) 0.0057(10) 0.0222(11) -0.0037(10)
C42 0.0209(11) 0.0227(11) 0.0421(13) -0.0021(10) 0.0112(10) -0.0028(9)
C41 0.0263(11) 0.0211(10) 0.0281(11) 0.0036(9) 0.0060(9) 0.0029(9)
C46 0.0201(10) 0.0292(11) 0.0171(9) 0.0049(9) 0.0041(8) 0.0001(9)
C47 0.0221(11) 0.0341(12) 0.0175(10) 0.0011(9) 0.0049(8) 0.0041(9)
C48 0.0275(12) 0.0397(13) 0.0199(10) -0.0065(10) 0.0039(9) -0.0071(10)
C49 0.0182(11) 0.0545(15) 0.0182(10) 0.0000(10) -0.0002(8) -0.0053(11)
C50 0.0188(11) 0.0434(14) 0.0256(11) 0.0113(10) 0.0032(9) 0.0062(10)
C51 0.0222(11) 0.0284(12) 0.0235(10) 0.0062(9) 0.0044(8) -0.0005(9)
C2 0.0184(10) 0.0182(10) 0.0154(9) 0.0022(8) -0.0004(8) -0.0043(8)
C1 0.0161(9) 0.0218(10) 0.0146(9) -0.0004(8) 0.0013(7) -0.0013(8)
C3 0.0197(10) 0.0198(10) 0.0164(9) 0.0032(8) -0.0011(8) 0.0004(8)
C52 0.0197(10) 0.0217(10) 0.0200(10) 0.0055(8) -0.0022(8) 0.0051(8)
C53 0.0221(10) 0.0230(11) 0.0295(11) 0.0029(9) 0.0034(9) 0.0013(9)
C54 0.0353(13) 0.0248(12) 0.0346(12) -0.0067(10) 0.0024(10) 0.0048(10)
C55 0.0333(12) 0.0384(13) 0.0255(11) -0.0074(10) 0.0086(10) 0.0086(11)
C56 0.0223(11) 0.0323(12) 0.0229(10) 0.0051(9) 0.0047(8) 0.0040(9)
C57 0.0232(10) 0.0207(10) 0.0198(10) 0.0016(9) 0.0003(8) 0.0014(9)
C10 0.0219(10) 0.0208(10) 0.0170(9) 0.0029(8) 0.0051(8) 0.0036(8)
C15 0.0241(11) 0.0279(11) 0.0159(9) 0.0056(9) 0.0035(8) 0.0012(9)
C14 0.0205(10) 0.0403(13) 0.0208(10) 0.0059(10) 0.0059(8) 0.0034(10)
C13 0.0316(12) 0.0351(12) 0.0245(11) 0.0053(10) 0.0133(9) 0.0109(10)
C12 0.0323(12) 0.0299(12) 0.0176(10) 0.0011(9) 0.0074(9) 0.0042(10)
C11 0.0262(11) 0.0245(11) 0.0144(9) 0.0036(8) 0.0038(8) 0.0010(9)
C28 0.0255(11) 0.0309(12) 0.0181(10) -0.0071(9) 0.0025(8) 0.0028(9)
C29 0.0296(12) 0.0409(14) 0.0415(13) -0.0039(12) -0.0002(10) -0.0012(11)
C30 0.0313(13) 0.0609(17) 0.0191(11) -0.0034(11) -0.0029(9) 0.0078(12)
C31 0.0199(10) 0.0391(13) 0.0234(11) -0.0018(10) 0.0033(8) 0.0002(10)
C33 0.0257(12) 0.0455(14) 0.0337(12) 0.0013(11) -0.0021(10) -0.0031(11)
C32 0.0275(12) 0.0549(15) 0.0204(11) 0.0014(11) 0.0010(9) -0.0009(11)
C22 0.0195(10) 0.0240(10) 0.0158(9) 0.0041(8) 0.0048(8) 0.0078(8)
C27 0.0239(11) 0.0249(11) 0.0177(10) 0.0029(9) 0.0008(8) 0.0077(9)
C26 0.0290(11) 0.0361(12) 0.0154(10) 0.0008(9) 0.0024(8) 0.0131(10)
C25 0.0271(12) 0.0430(14) 0.0230(11) 0.0103(10) 0.0102(9) 0.0085(10)
C24 0.0232(11) 0.0327(12) 0.0267(11) 0.0108(10) 0.0074(9) 0.0021(9)
C23 0.0196(10) 0.0266(11) 0.0234(10) 0.0057(9) 0.0035(8) 0.0042(9)
C34 0.0233(11) 0.0248(11) 0.0288(11) 0.0009(9) 0.0072(9) -0.0029(9)
C35 0.0299(12) 0.0277(12) 0.0450(13) 0.0031(11) 0.0075(10) -0.0031(10)
C36 0.0268(12) 0.0337(13) 0.0346(12) -0.0005(10) 0.0040(10) -0.0029(10)
C37 0.0288(11) 0.0259(11) 0.0200(10) -0.0010(9) -0.0012(9) 0.0046(9)
C38 0.0409(14) 0.0350(13) 0.0327(12) -0.0110(11) -0.0014(10) -0.0005(11)
C39 0.0287(12) 0.0335(12) 0.0265(11) -0.0022(10) 0.0009(9) -0.0025(10)
C4 0.0233(10) 0.0218(10) 0.0195(10) 0.0035(8) 0.0051(8) 0.0049(9)
C9 0.0223(11) 0.0315(12) 0.0278(11) 0.0091(10) 0.0047(9) 0.0040(9)
C8 0.0291(12) 0.0362(13) 0.0400(13) 0.0149(11) 0.0171(10) 0.0066(10)
C7 0.0457(14) 0.0375(13) 0.0247(11) 0.0109(10) 0.0167(10) 0.0111(11)
C6 0.0376(13) 0.0419(14) 0.0183(10) 0.0061(10) 0.0008(9) 0.0097(11)
C5 0.0266(11) 0.0320(12) 0.0218(10) 0.0014(9) 0.0041(9) 0.0022(10)
C16 0.0162(10) 0.0222(10) 0.0180(9) 0.0029(8) 0.0032(8) -0.0010(8)
C21 0.0209(10) 0.0235(11) 0.0215(10) 0.0012(9) 0.0045(8) 0.0024(9)
C20 0.0257(11) 0.0289(11) 0.0178(10) 0.0067(9) 0.0037(8) 0.0036(9)
C19 0.0270(11) 0.0222(11) 0.0247(10) 0.0071(9) 0.0035(9) -0.0004(9)
C18 0.0269(11) 0.0187(10) 0.0287(11) 0.0001(9) 0.0042(9) 0.0011(9)
C17 0.0217(10) 0.0244(11) 0.0188(10) -0.0005(9) 0.0021(8) -0.0042(9)
B1 0.0200(11) 0.0202(11) 0.0206(11) 0.0019(10) 0.0041(9) 0.0002(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
F11 C53 1.349(2) . ?
F12 C54 1.346(2) . ?
F15 C57 1.352(2) . ?
F13 C55 1.348(2) . ?
F14 C56 1.344(2) . ?
F6 C47 1.357(2) . ?
F7 C48 1.345(2) . ?
F10 C51 1.358(2) . ?
F8 C49 1.340(2) . ?
F9 C50 1.348(2) . ?
F5 C45 1.357(2) . ?
F4 C44 1.346(2) . ?
F1 C41 1.358(2) . ?
F3 C43 1.344(2) . ?
F2 C42 1.351(2) . ?
N1 C2 1.417(2) . ?
N1 C1 1.358(2) . ?
N1 C22 1.460(2) . ?
N2 C1 1.349(2) . ?
N2 C3 1.402(2) . ?
N2 C10 1.455(2) . ?
C40 C45 1.396(3) . ?
C40 C41 1.397(3) . ?
C40 B1 1.663(3) . ?
C45 C44 1.378(3) . ?
C44 C43 1.369(3) . ?
C43 C42 1.380(3) . ?
C42 C41 1.369(3) . ?
C46 C47 1.390(3) . ?
C46 C51 1.399(3) . ?
C46 B1 1.666(3) . ?
C47 C48 1.379(3) . ?
C48 C49 1.375(3) . ?
C49 C50 1.370(3) . ?
C50 C51 1.379(3) . ?
C2 C3 1.370(3) . ?
C2 B1 1.674(3) . ?
C1 C16 1.493(3) . ?
C3 C4 1.484(3) . ?
C52 C53 1.388(3) . ?
C52 C57 1.389(3) . ?
C52 B1 1.683(3) . ?
C53 C54 1.391(3) . ?
C54 C55 1.366(3) . ?
C55 C56 1.369(3) . ?
C56 C57 1.383(3) . ?
C10 C15 1.396(3) . ?
C10 C11 1.408(3) . ?
C15 C14 1.394(3) . ?
C15 C31 1.526(3) . ?
C14 C13 1.382(3) . ?
C13 C12 1.386(3) . ?
C12 C11 1.386(3) . ?
C11 C28 1.522(3) . ?
C28 C29 1.525(3) . ?
C28 C30 1.535(3) . ?
C31 C33 1.528(3) . ?
C31 C32 1.530(3) . ?
C22 C27 1.409(3) . ?
C22 C23 1.402(3) . ?
C27 C26 1.397(3) . ?
C27 C37 1.529(3) . ?
C26 C25 1.386(3) . ?
C25 C24 1.371(3) . ?
C24 C23 1.400(3) . ?
C23 C34 1.523(3) . ?
C34 C35 1.535(3) . ?
C34 C36 1.533(3) . ?
C37 C38 1.530(3) . ?
C37 C39 1.533(3) . ?
C4 C9 1.401(3) . ?
C4 C5 1.391(3) . ?
C9 C8 1.387(3) . ?
C8 C7 1.380(3) . ?
C7 C6 1.389(3) . ?
C6 C5 1.389(3) . ?
C16 C21 1.405(3) . ?
C16 C17 1.393(3) . ?
C21 C20 1.386(3) . ?
C20 C19 1.380(3) . ?
C19 C18 1.386(3) . ?
C18 C17 1.385(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
C2 N1 C22 127.83(15) . . ?
C1 N1 C2 110.92(14) . . ?
C1 N1 C22 121.08(15) . . ?
C1 N2 C3 109.01(15) . . ?
C1 N2 C10 125.43(16) . . ?
C3 N2 C10 125.49(15) . . ?
C45 C40 C41 111.83(18) . . ?
C45 C40 B1 126.65(18) . . ?
C41 C40 B1 121.31(17) . . ?
F5 C45 C40 121.64(18) . . ?
F5 C45 C44 113.59(18) . . ?
C44 C45 C40 124.7(2) . . ?
F4 C44 C45 119.4(2) . . ?
F4 C44 C43 120.40(19) . . ?
C43 C44 C45 120.1(2) . . ?
F3 C43 C44 121.1(2) . . ?
F3 C43 C42 120.5(2) . . ?
C44 C43 C42 118.28(19) . . ?
F2 C42 C43 119.68(18) . . ?
F2 C42 C41 120.66(19) . . ?
C41 C42 C43 119.6(2) . . ?
F1 C41 C40 119.74(17) . . ?
F1 C41 C42 114.82(18) . . ?
C42 C41 C40 125.39(19) . . ?
C47 C46 C51 112.16(17) . . ?
C47 C46 B1 127.73(17) . . ?
C51 C46 B1 119.62(18) . . ?
F6 C47 C46 120.54(17) . . ?
F6 C47 C48 114.72(18) . . ?
C48 C47 C46 124.73(19) . . ?
F7 C48 C47 120.1(2) . . ?
F7 C48 C49 119.97(19) . . ?
C49 C48 C47 119.9(2) . . ?
F8 C49 C48 121.3(2) . . ?
F8 C49 C50 120.1(2) . . ?
C50 C49 C48 118.69(19) . . ?
F9 C50 C49 119.17(19) . . ?
F9 C50 C51 121.3(2) . . ?
C49 C50 C51 119.5(2) . . ?
F10 C51 C46 119.18(17) . . ?
F10 C51 C50 115.79(18) . . ?
C50 C51 C46 125.0(2) . . ?
N1 C2 B1 130.26(16) . . ?
C3 C2 N1 104.28(16) . . ?
C3 C2 B1 125.44(16) . . ?
N1 C1 C16 127.83(16) . . ?
N2 C1 N1 106.86(16) . . ?
N2 C1 C16 125.31(17) . . ?
N2 C3 C4 118.95(17) . . ?
C2 C3 N2 108.90(16) . . ?
C2 C3 C4 132.14(18) . . ?
C53 C52 C57 112.28(18) . . ?
C53 C52 B1 126.43(18) . . ?
C57 C52 B1 120.62(17) . . ?
F11 C53 C52 121.94(18) . . ?
F11 C53 C54 114.08(18) . . ?
C52 C53 C54 123.98(19) . . ?
F12 C54 C53 119.6(2) . . ?
F12 C54 C55 119.88(19) . . ?
C55 C54 C53 120.5(2) . . ?
F13 C55 C54 121.0(2) . . ?
F13 C55 C56 120.7(2) . . ?
C54 C55 C56 118.37(19) . . ?
F14 C56 C55 119.91(18) . . ?
F14 C56 C57 120.74(19) . . ?
C55 C56 C57 119.35(19) . . ?
F15 C57 C52 120.82(17) . . ?
F15 C57 C56 113.69(17) . . ?
C56 C57 C52 125.49(19) . . ?
C15 C10 N2 119.15(17) . . ?
C15 C10 C11 123.36(18) . . ?
C11 C10 N2 117.41(16) . . ?
C10 C15 C31 123.55(18) . . ?
C14 C15 C10 117.00(18) . . ?
C14 C15 C31 119.43(18) . . ?
C13 C14 C15 121.03(19) . . ?
C14 C13 C12 120.44(19) . . ?
C13 C12 C11 121.19(19) . . ?
C10 C11 C28 122.63(17) . . ?
C12 C11 C10 116.86(18) . . ?
C12 C11 C28 120.51(18) . . ?
C11 C28 C29 113.16(17) . . ?
C11 C28 C30 111.40(17) . . ?
C29 C28 C30 110.12(18) . . ?
C15 C31 C33 112.09(17) . . ?
C15 C31 C32 111.45(18) . . ?
C33 C31 C32 109.14(17) . . ?
C27 C22 N1 118.61(17) . . ?
C23 C22 N1 117.92(16) . . ?
C23 C22 C27 123.36(17) . . ?
C22 C27 C37 122.99(17) . . ?
C26 C27 C22 116.09(18) . . ?
C26 C27 C37 120.91(18) . . ?
C25 C26 C27 121.79(19) . . ?
C24 C25 C26 120.43(19) . . ?
C25 C24 C23 121.1(2) . . ?
C22 C23 C34 124.85(17) . . ?
C24 C23 C22 117.09(18) . . ?
C24 C23 C34 118.06(18) . . ?
C23 C34 C35 110.52(17) . . ?
C23 C34 C36 112.16(17) . . ?
C36 C34 C35 109.09(17) . . ?
C27 C37 C38 112.88(17) . . ?
C27 C37 C39 114.57(17) . . ?
C38 C37 C39 107.68(17) . . ?
C9 C4 C3 119.95(17) . . ?
C5 C4 C3 121.93(18) . . ?
C5 C4 C9 118.12(18) . . ?
C8 C9 C4 121.01(19) . . ?
C7 C8 C9 120.1(2) . . ?
C8 C7 C6 119.78(19) . . ?
C7 C6 C5 120.2(2) . . ?
C6 C5 C4 120.8(2) . . ?
C21 C16 C1 121.31(17) . . ?
C17 C16 C1 120.70(16) . . ?
C17 C16 C21 117.97(18) . . ?
C20 C21 C16 120.38(19) . . ?
C19 C20 C21 121.11(18) . . ?
C20 C19 C18 118.88(19) . . ?
C17 C18 C19 120.70(19) . . ?
C18 C17 C16 120.94(18) . . ?
C40 B1 C46 110.97(16) . . ?
C40 B1 C2 104.87(15) . . ?
C40 B1 C52 111.57(16) . . ?
C46 B1 C2 111.47(16) . . ?
C46 B1 C52 102.34(15) . . ?
C2 B1 C52 115.80(15) . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.500 449.1 144.3 ?
2 0.500 1.000 0.000 449.1 144.3 ?