# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
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data_kjf136x_a
_database_code_depnum_ccdc_archive 'CCDC 1841032'
_audit_update_record
;
2018-05-02 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;
_audit_creation_date 2018-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic
Tris[5-(4-allyloxytetrafluorophenyl)diprrin]indium(III)
_chemical_formula_moiety 'C54 H33 F12 In1 N6 O3'
_chemical_formula_sum 'C54 H33 F12 In N6 O3'
_chemical_formula_weight 1156.68
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system trigonal
_space_group_IT_number 148
_space_group_name_H-M_alt 'R -3'
_space_group_name_Hall '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
_cell_length_a 23.433(3)
_cell_length_b 23.433(3)
_cell_length_c 15.332(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 7291(3)
_cell_formula_units_Z 6
_cell_measurement_reflns_used 6529
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 23.92
_cell_measurement_theta_min 2.84
_shelx_estimated_absorpt_T_max 0.983
_shelx_estimated_absorpt_T_min 0.759
_exptl_absorpt_coefficient_mu 0.585
_exptl_absorpt_correction_T_max 0.7453
_exptl_absorpt_correction_T_min 0.6478
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0762 before and 0.0590 after correction. The Ratio of minimum to maximum transmission is 0.8692. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light orange'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.581
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Needle
_exptl_crystal_F_000 3480
_exptl_crystal_preparation ?
_exptl_crystal_recrystallization_method
'The material was recrystallised from DCM by slow evaporation'
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.03
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0954
_diffrn_reflns_av_unetI/netI 0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 48936
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 26.291
_diffrn_reflns_theta_min 2.407
_diffrn_ambient_temperature 100(2)
_diffrn_detector 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device 'Kappa diffractometer'
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_collimation '0.5 mm double-pinhole'
_diffrn_radiation_detector 'Bruker PHOTON 50'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'standard sealed X-ray tube'
_diffrn_source_type 'Siemens, KFF Mo 2K -90 C'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2500
_reflns_number_total 3274
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection 'APEX 3 (Bruker, 2016) '
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XT (Sheldrick, 2015)'
_refine_diff_density_max 0.333
_refine_diff_density_min -0.424
_refine_diff_density_rms 0.069
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.027
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 229
_refine_ls_number_reflns 3274
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0533
_refine_ls_R_factor_gt 0.0308
_refine_ls_restrained_S_all 1.027
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+15.7543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0591
_refine_ls_wR_factor_ref 0.0656
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C18(H18)
2.c X=CH2 refined with riding coordinates:
C19(H19A,H19B)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.85713(11) 0.45205(12) 0.43795(16) 0.0195(5) Uani 1 1 d . . . . .
H1 H 0.8981 0.4907 0.4265 0.023 Uiso 1 1 calc R . . . .
C2 C 0.83028(12) 0.39456(12) 0.39183(16) 0.0199(5) Uani 1 1 d . . . . .
H2 H 0.8488 0.3851 0.3427 0.024 Uiso 1 1 calc R . . . .
C3 C 0.76951(12) 0.35211(12) 0.43194(15) 0.0180(5) Uani 1 1 d . . . . .
H3 H 0.7402 0.3084 0.4127 0.022 Uiso 1 1 calc R . . . .
C5 C 0.69871(12) 0.43474(12) 0.73483(16) 0.0187(5) Uani 1 1 d . . . . .
H5 H 0.6575 0.4048 0.7604 0.022 Uiso 1 1 calc R . . . .
C6 C 0.74382(12) 0.49609(12) 0.77097(16) 0.0195(5) Uani 1 1 d . . . . .
H6 H 0.7392 0.5143 0.8241 0.023 Uiso 1 1 calc R . . . .
C7 C 0.79591(12) 0.52440(12) 0.71417(16) 0.0192(5) Uani 1 1 d . . . . .
H7 H 0.8343 0.5664 0.7202 0.023 Uiso 1 1 calc R . . . .
C8 C 0.82189(11) 0.48793(11) 0.57240(16) 0.0168(5) Uani 1 1 d . . . . .
C9 C 0.81234(11) 0.44324(11) 0.50642(15) 0.0160(5) Uani 1 1 d . . . . .
C10 C 0.78174(11) 0.47933(11) 0.64483(15) 0.0160(5) Uani 1 1 d . . . . .
C11 C 0.88373(11) 0.55365(11) 0.56672(16) 0.0161(5) Uani 1 1 d . . . . .
C12 C 0.88465(12) 0.60695(12) 0.52605(17) 0.0203(6) Uani 1 1 d . . . . .
C13 C 0.94079(12) 0.66763(11) 0.52343(17) 0.0220(6) Uani 1 1 d . . . . .
C14 C 0.99851(11) 0.67912(11) 0.56311(16) 0.0200(5) Uani 1 1 d . . . . .
C15 C 0.99766(11) 0.62634(12) 0.60380(17) 0.0213(5) Uani 1 1 d . . . . .
C16 C 0.94197(12) 0.56508(11) 0.60408(16) 0.0196(5) Uani 1 1 d . . . . .
C17 C 1.05545(13) 0.79191(12) 0.60623(17) 0.0263(6) Uani 1 1 d . . . . .
H17A H 1.0206 0.7994 0.5822 0.032 Uiso 1 1 calc R . . . .
H17B H 1.0983 0.8327 0.5976 0.032 Uiso 1 1 calc R . . . .
C18 C 1.04394(14) 0.77807(13) 0.70114(19) 0.0291(7) Uani 1 1 d . . . . .
H18 H 1.0724 0.7673 0.7321 0.035 Uiso 1 1 calc R . . . .
C19 C 0.99680(15) 0.77988(14) 0.7445(2) 0.0364(7) Uani 1 1 d . . . . .
H19A H 0.9676 0.7905 0.7153 0.044 Uiso 1 1 calc R . . . .
H19B H 0.9918 0.7706 0.8052 0.044 Uiso 1 1 calc R . . . .
F1 F 0.82997(7) 0.59917(7) 0.48720(11) 0.0333(4) Uani 1 1 d . . . . .
F2 F 0.93978(8) 0.71729(7) 0.48006(11) 0.0340(4) Uani 1 1 d . . . . .
F3 F 1.05230(7) 0.63496(7) 0.64457(11) 0.0348(4) Uani 1 1 d . . . . .
F4 F 0.94456(7) 0.51517(7) 0.64293(10) 0.0307(4) Uani 1 1 d . . . . .
In1 In 0.6667 0.3333 0.58002(2) 0.01447(8) Uani 1 3 d S T P . .
N1 N 0.75770(9) 0.37996(10) 0.49958(13) 0.0163(4) Uani 1 1 d . . . . .
N2 N 0.72076(9) 0.42369(9) 0.66029(13) 0.0158(4) Uani 1 1 d . . . . .
O1 O 1.05566(8) 0.73803(8) 0.55871(12) 0.0276(4) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0145(11) 0.0241(13) 0.0189(13) 0.0039(11) 0.0012(10) 0.0090(10)
C2 0.0189(12) 0.0297(14) 0.0166(13) -0.0024(11) -0.0001(10) 0.0163(11)
C3 0.0195(12) 0.0205(12) 0.0167(13) -0.0055(10) -0.0030(10) 0.0120(10)
C5 0.0207(12) 0.0214(12) 0.0166(13) 0.0011(10) 0.0030(10) 0.0126(11)
C6 0.0266(14) 0.0206(12) 0.0152(13) -0.0032(10) -0.0029(11) 0.0147(11)
C7 0.0207(12) 0.0176(12) 0.0190(14) -0.0024(10) -0.0021(10) 0.0092(10)
C8 0.0153(11) 0.0142(11) 0.0209(13) 0.0028(10) -0.0004(10) 0.0074(10)
C9 0.0148(11) 0.0173(12) 0.0160(13) 0.0020(10) 0.0010(10) 0.0081(10)
C10 0.0165(11) 0.0141(11) 0.0174(13) 0.0010(10) -0.0015(10) 0.0077(10)
C11 0.0161(12) 0.0155(12) 0.0170(13) -0.0016(10) 0.0013(10) 0.0081(10)
C12 0.0172(12) 0.0198(13) 0.0243(15) -0.0018(11) -0.0045(11) 0.0095(11)
C13 0.0269(13) 0.0149(12) 0.0241(15) 0.0034(10) 0.0003(11) 0.0104(11)
C14 0.0174(12) 0.0141(12) 0.0244(14) -0.0013(10) 0.0047(10) 0.0047(10)
C15 0.0133(12) 0.0244(13) 0.0270(15) -0.0035(11) -0.0034(10) 0.0100(10)
C16 0.0215(13) 0.0166(12) 0.0226(14) 0.0016(10) 0.0004(11) 0.0110(10)
C17 0.0255(14) 0.0139(12) 0.0302(16) -0.0023(11) -0.0049(12) 0.0028(11)
C18 0.0303(15) 0.0240(14) 0.0310(17) 0.0008(12) -0.0102(13) 0.0120(13)
C19 0.050(2) 0.0355(17) 0.0295(17) 0.0002(14) -0.0035(15) 0.0259(16)
F1 0.0234(8) 0.0240(8) 0.0495(11) 0.0030(7) -0.0159(7) 0.0097(7)
F2 0.0372(9) 0.0175(8) 0.0433(10) 0.0064(7) -0.0111(8) 0.0107(7)
F3 0.0178(8) 0.0298(8) 0.0557(11) -0.0009(8) -0.0117(7) 0.0109(7)
F4 0.0304(8) 0.0204(8) 0.0433(10) 0.0050(7) -0.0100(7) 0.0141(7)
In1 0.01379(10) 0.01379(10) 0.01585(16) 0.000 0.000 0.00689(5)
N1 0.0152(10) 0.0161(10) 0.0169(11) -0.0013(9) 0.0004(8) 0.0073(9)
N2 0.0159(10) 0.0141(10) 0.0176(11) 0.0005(8) 0.0009(8) 0.0075(8)
O1 0.0175(9) 0.0158(9) 0.0397(12) -0.0016(8) 0.0049(8) 0.0009(7)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9500 . ?
C1 C2 1.365(3) . ?
C1 C9 1.425(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.407(3) . ?
C3 H3 0.9500 . ?
C3 N1 1.326(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.404(3) . ?
C5 N2 1.332(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.371(3) . ?
C7 H7 0.9500 . ?
C7 C10 1.416(3) . ?
C8 C9 1.391(3) . ?
C8 C10 1.403(3) . ?
C8 C11 1.499(3) . ?
C9 N1 1.397(3) . ?
C10 N2 1.391(3) . ?
C11 C12 1.386(3) . ?
C11 C16 1.377(3) . ?
C12 C13 1.372(3) . ?
C12 F1 1.340(3) . ?
C13 C14 1.381(3) . ?
C13 F2 1.351(3) . ?
C14 C15 1.376(3) . ?
C14 O1 1.362(3) . ?
C15 C16 1.375(3) . ?
C15 F3 1.346(3) . ?
C16 F4 1.341(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.486(4) . ?
C17 O1 1.460(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.308(4) . ?
C19 H19A 0.9500 . ?
C19 H19B 0.9500 . ?
In1 N1 2.2213(19) 2_655 ?
In1 N1 2.2213(19) 3_665 ?
In1 N1 2.221(2) . ?
In1 N2 2.218(2) . ?
In1 N2 2.218(2) 2_655 ?
In1 N2 2.218(2) 3_665 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 126.4 . . ?
C2 C1 C9 107.2(2) . . ?
C9 C1 H1 126.4 . . ?
C1 C2 H2 127.0 . . ?
C1 C2 C3 106.0(2) . . ?
C3 C2 H2 127.0 . . ?
C2 C3 H3 123.8 . . ?
N1 C3 C2 112.4(2) . . ?
N1 C3 H3 123.8 . . ?
C6 C5 H5 124.1 . . ?
N2 C5 H5 124.1 . . ?
N2 C5 C6 111.8(2) . . ?
C5 C6 H6 127.0 . . ?
C7 C6 C5 106.1(2) . . ?
C7 C6 H6 127.0 . . ?
C6 C7 H7 126.4 . . ?
C6 C7 C10 107.2(2) . . ?
C10 C7 H7 126.4 . . ?
C9 C8 C10 128.6(2) . . ?
C9 C8 C11 116.1(2) . . ?
C10 C8 C11 115.3(2) . . ?
C8 C9 C1 126.7(2) . . ?
C8 C9 N1 124.8(2) . . ?
N1 C9 C1 108.5(2) . . ?
C8 C10 C7 126.6(2) . . ?
N2 C10 C7 108.6(2) . . ?
N2 C10 C8 124.8(2) . . ?
C12 C11 C8 121.5(2) . . ?
C16 C11 C8 122.0(2) . . ?
C16 C11 C12 116.4(2) . . ?
C13 C12 C11 121.4(2) . . ?
F1 C12 C11 119.6(2) . . ?
F1 C12 C13 118.9(2) . . ?
C12 C13 C14 121.8(2) . . ?
F2 C13 C12 119.1(2) . . ?
F2 C13 C14 119.1(2) . . ?
C15 C14 C13 116.9(2) . . ?
O1 C14 C13 123.1(2) . . ?
O1 C14 C15 119.9(2) . . ?
C16 C15 C14 121.3(2) . . ?
F3 C15 C14 119.4(2) . . ?
F3 C15 C16 119.4(2) . . ?
C15 C16 C11 122.2(2) . . ?
F4 C16 C11 119.2(2) . . ?
F4 C16 C15 118.6(2) . . ?
H17A C17 H17B 107.9 . . ?
C18 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
O1 C17 H17A 109.2 . . ?
O1 C17 H17B 109.2 . . ?
O1 C17 C18 112.3(2) . . ?
C17 C18 H18 118.1 . . ?
C19 C18 C17 123.7(3) . . ?
C19 C18 H18 118.1 . . ?
C18 C19 H19A 120.0 . . ?
C18 C19 H19B 120.0 . . ?
H19A C19 H19B 120.0 . . ?
N1 In1 N1 92.16(7) . 2_655 ?
N1 In1 N1 92.16(7) 3_665 . ?
N1 In1 N1 92.16(7) 3_665 2_655 ?
N2 In1 N1 83.61(7) 2_655 2_655 ?
N2 In1 N1 92.36(7) 3_665 . ?
N2 In1 N1 173.92(7) 2_655 . ?
N2 In1 N1 92.36(7) . 2_655 ?
N2 In1 N1 83.61(7) . . ?
N2 In1 N1 173.92(7) 3_665 2_655 ?
N2 In1 N1 83.61(7) 3_665 3_665 ?
N2 In1 N1 173.92(7) . 3_665 ?
N2 In1 N1 92.36(7) 2_655 3_665 ?
N2 In1 N2 92.19(7) . 2_655 ?
N2 In1 N2 92.19(7) 3_665 2_655 ?
N2 In1 N2 92.19(7) 3_665 . ?
C3 N1 C9 105.96(19) . . ?
C3 N1 In1 125.28(16) . . ?
C9 N1 In1 128.73(15) . . ?
C5 N2 C10 106.3(2) . . ?
C5 N2 In1 124.72(16) . . ?
C10 N2 In1 128.98(15) . . ?
C14 O1 C17 115.16(19) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C17 H17A F2 0.99 2.47 3.067(3) 118.5 .
C17 H17B F4 0.99 2.32 3.091(3) 134.1 14_566
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 N1 -0.1(3) . . . . ?
C1 C9 N1 C3 1.0(3) . . . . ?
C1 C9 N1 In1 -177.20(15) . . . . ?
C2 C1 C9 C8 175.7(2) . . . . ?
C2 C1 C9 N1 -1.1(3) . . . . ?
C2 C3 N1 C9 -0.5(3) . . . . ?
C2 C3 N1 In1 177.73(15) . . . . ?
C5 C6 C7 C10 -0.6(3) . . . . ?
C6 C5 N2 C10 -1.0(3) . . . . ?
C6 C5 N2 In1 179.81(15) . . . . ?
C6 C7 C10 C8 -179.5(2) . . . . ?
C6 C7 C10 N2 0.0(3) . . . . ?
C7 C10 N2 C5 0.6(2) . . . . ?
C7 C10 N2 In1 179.76(15) . . . . ?
C8 C9 N1 C3 -175.9(2) . . . . ?
C8 C9 N1 In1 5.9(3) . . . . ?
C8 C10 N2 C5 -179.9(2) . . . . ?
C8 C10 N2 In1 -0.7(3) . . . . ?
C8 C11 C12 C13 177.8(2) . . . . ?
C8 C11 C12 F1 -3.2(4) . . . . ?
C8 C11 C16 C15 -175.8(2) . . . . ?
C8 C11 C16 F4 3.5(4) . . . . ?
C9 C1 C2 C3 0.7(3) . . . . ?
C9 C8 C10 C7 174.7(2) . . . . ?
C9 C8 C10 N2 -4.7(4) . . . . ?
C9 C8 C11 C12 93.4(3) . . . . ?
C9 C8 C11 C16 -89.0(3) . . . . ?
C10 C8 C9 C1 -174.3(2) . . . . ?
C10 C8 C9 N1 2.0(4) . . . . ?
C10 C8 C11 C12 -87.7(3) . . . . ?
C10 C8 C11 C16 90.0(3) . . . . ?
C11 C8 C9 C1 4.5(4) . . . . ?
C11 C8 C9 N1 -179.3(2) . . . . ?
C11 C8 C10 C7 -4.1(3) . . . . ?
C11 C8 C10 N2 176.5(2) . . . . ?
C11 C12 C13 C14 -1.8(4) . . . . ?
C11 C12 C13 F2 177.4(2) . . . . ?
C12 C11 C16 C15 2.0(4) . . . . ?
C12 C11 C16 F4 -178.7(2) . . . . ?
C12 C13 C14 C15 1.5(4) . . . . ?
C12 C13 C14 O1 177.3(2) . . . . ?
C13 C14 C15 C16 0.5(4) . . . . ?
C13 C14 C15 F3 -179.1(2) . . . . ?
C13 C14 O1 C17 69.1(3) . . . . ?
C14 C15 C16 C11 -2.3(4) . . . . ?
C14 C15 C16 F4 178.4(2) . . . . ?
C15 C14 O1 C17 -115.2(3) . . . . ?
C16 C11 C12 C13 0.1(4) . . . . ?
C16 C11 C12 F1 179.1(2) . . . . ?
C18 C17 O1 C14 60.7(3) . . . . ?
F1 C12 C13 C14 179.2(2) . . . . ?
F1 C12 C13 F2 -1.6(4) . . . . ?
F2 C13 C14 C15 -177.8(2) . . . . ?
F2 C13 C14 O1 -2.0(4) . . . . ?
F3 C15 C16 C11 177.3(2) . . . . ?
F3 C15 C16 F4 -2.0(4) . . . . ?
N2 C5 C6 C7 1.0(3) . . . . ?
O1 C14 C15 C16 -175.4(2) . . . . ?
O1 C14 C15 F3 5.0(4) . . . . ?
O1 C17 C18 C19 -124.8(3) . . . . ?
_shelx_res_file
;
kjf136x_a.res created by SHELXL-2014/7
TITL kjf136x_a.res in R-3
REM Old TITL kjf136x in R-3
REM SHELXT solution in R-3
REM R1 0.089, Rweak 0.007, Alpha 0.019, Orientation as input
REM Formula found by SHELXT: C54 N9 F12 In
CELL 0.71073 23.4325 23.4325 15.3319 90 90 120
ZERR 6 0.0027 0.0027 0.0047 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H F In N O
UNIT 324 198 72 6 36 18
EQIV $1 0.667+Y,1.333-X+Y,1.333-Z
L.S. 10
PLAN 20
SIZE 0.03 0.03 0.5
TEMP -173(2)
HTAB C17 F2
HTAB C17 F4_$1
BOND $H
HTAB
WPDB
MORE -1
CONF
fmap 2
acta 52
REM
REM
REM
WGHT 0.024300 15.754300
FVAR 0.12268
C1 1 0.857135 0.452055 0.437946 11.00000 0.01452 0.02410 =
0.01886 0.00386 0.00122 0.00897
AFIX 43
H1 2 0.898057 0.490730 0.426516 11.00000 -1.20000
AFIX 0
C2 1 0.830279 0.394561 0.391828 11.00000 0.01888 0.02974 =
0.01658 -0.00243 -0.00013 0.01627
AFIX 43
H2 2 0.848845 0.385134 0.342657 11.00000 -1.20000
AFIX 0
C3 1 0.769512 0.352113 0.431940 11.00000 0.01953 0.02048 =
0.01673 -0.00546 -0.00304 0.01204
AFIX 43
H3 2 0.740247 0.308436 0.412744 11.00000 -1.20000
AFIX 0
C5 1 0.698711 0.434736 0.734833 11.00000 0.02071 0.02141 =
0.01658 0.00114 0.00296 0.01256
AFIX 43
H5 2 0.657476 0.404753 0.760440 11.00000 -1.20000
AFIX 0
C6 1 0.743825 0.496089 0.770970 11.00000 0.02663 0.02060 =
0.01521 -0.00316 -0.00292 0.01468
AFIX 43
H6 2 0.739183 0.514292 0.824051 11.00000 -1.20000
AFIX 0
C7 1 0.795909 0.524400 0.714172 11.00000 0.02065 0.01758 =
0.01899 -0.00236 -0.00207 0.00924
AFIX 43
H7 2 0.834346 0.566423 0.720195 11.00000 -1.20000
AFIX 0
C8 1 0.821888 0.487928 0.572397 11.00000 0.01531 0.01416 =
0.02092 0.00280 -0.00045 0.00741
C9 1 0.812343 0.443241 0.506424 11.00000 0.01479 0.01731 =
0.01598 0.00201 0.00100 0.00808
C10 1 0.781743 0.479325 0.644831 11.00000 0.01653 0.01406 =
0.01741 0.00098 -0.00147 0.00770
C11 1 0.883732 0.553645 0.566715 11.00000 0.01608 0.01553 =
0.01699 -0.00157 0.00128 0.00813
C12 1 0.884651 0.606947 0.526052 11.00000 0.01717 0.01978 =
0.02433 -0.00178 -0.00451 0.00949
C13 1 0.940791 0.667626 0.523428 11.00000 0.02694 0.01488 =
0.02406 0.00341 0.00033 0.01038
C14 1 0.998510 0.679118 0.563111 11.00000 0.01736 0.01410 =
0.02442 -0.00128 0.00468 0.00467
C15 1 0.997662 0.626338 0.603803 11.00000 0.01330 0.02438 =
0.02703 -0.00354 -0.00339 0.01001
C16 1 0.941970 0.565085 0.604079 11.00000 0.02152 0.01661 =
0.02264 0.00156 0.00041 0.01101
C17 1 1.055454 0.791914 0.606234 11.00000 0.02553 0.01387 =
0.03020 -0.00229 -0.00490 0.00276
AFIX 23
H17A 2 1.020560 0.799440 0.582157 11.00000 -1.20000
H17B 2 1.098301 0.832726 0.597564 11.00000 -1.20000
AFIX 0
C18 1 1.043943 0.778071 0.701135 11.00000 0.03027 0.02402 =
0.03096 0.00085 -0.01021 0.01196
AFIX 43
H18 2 1.072428 0.767298 0.732055 11.00000 -1.20000
AFIX 0
C19 1 0.996799 0.779880 0.744527 11.00000 0.05013 0.03555 =
0.02952 0.00021 -0.00348 0.02585
AFIX 93
H19A 2 0.967566 0.790510 0.715315 11.00000 -1.20000
H19B 2 0.991799 0.770563 0.805248 11.00000 -1.20000
AFIX 0
F1 3 0.829966 0.599174 0.487200 11.00000 0.02345 0.02401 =
0.04948 0.00305 -0.01587 0.00966
F2 3 0.939782 0.717295 0.480064 11.00000 0.03720 0.01750 =
0.04326 0.00640 -0.01113 0.01066
F3 3 1.052301 0.634964 0.644569 11.00000 0.01780 0.02976 =
0.05567 -0.00086 -0.01168 0.01092
F4 3 0.944555 0.515173 0.642931 11.00000 0.03044 0.02037 =
0.04330 0.00499 -0.01002 0.01410
IN1 4 0.666667 0.333333 0.580022 10.33333 0.01379 0.01379 =
0.01585 0.00000 0.00000 0.00689
N1 5 0.757697 0.379962 0.499584 11.00000 0.01517 0.01611 =
0.01694 -0.00133 0.00044 0.00732
N2 5 0.720758 0.423688 0.660292 11.00000 0.01589 0.01409 =
0.01756 0.00051 0.00089 0.00752
O1 6 1.055659 0.738030 0.558705 11.00000 0.01749 0.01579 =
0.03967 -0.00156 0.00493 0.00094
HKLF 4
REM kjf136x_a.res in R-3
REM R1 = 0.0308 for 2500 Fo > 4sig(Fo) and 0.0533 for all 3274 data
REM 229 parameters refined using 0 restraints
END
WGHT 0.0243 15.7547
REM Instructions for potential hydrogen bonds
EQIV $2 -x+2, -y+1, -z+1
HTAB C2 F3_$2
EQIV $3 -x+5/3, -y+4/3, -z+4/3
HTAB C6 F2_$3
HTAB C17 F2
HTAB C17 F4_$1
REM Highest difference peak 0.333, deepest hole -0.424, 1-sigma level 0.069
Q1 1 0.7072 0.3946 0.6218 11.00000 0.05 0.33
Q2 1 0.8043 0.4718 0.6220 11.00000 0.05 0.32
Q3 1 0.8821 0.5816 0.5533 11.00000 0.05 0.28
Q4 1 0.6567 0.4208 0.6412 11.00000 0.05 0.27
Q5 1 0.7929 0.4966 0.6856 11.00000 0.05 0.27
Q6 1 1.0341 0.7820 0.6523 11.00000 0.05 0.26
Q7 1 1.1253 0.8099 0.7028 11.00000 0.05 0.26
Q8 1 0.8056 0.4646 0.5364 11.00000 0.05 0.25
Q9 1 0.8265 0.4518 0.4623 11.00000 0.05 0.25
Q10 1 1.1012 0.7611 0.6015 11.00000 0.05 0.25
Q11 1 0.7291 0.3632 0.5345 11.00000 0.05 0.25
Q12 1 0.8905 0.5646 0.4383 11.00000 0.05 0.24
Q13 1 0.9645 0.6020 0.6243 11.00000 0.05 0.24
Q14 1 0.8672 0.5264 0.5546 11.00000 0.05 0.23
Q15 1 0.9430 0.6894 0.5045 11.00000 0.05 0.23
Q16 1 0.9648 0.6822 0.5686 11.00000 0.05 0.23
Q17 1 0.7982 0.3631 0.3982 11.00000 0.05 0.23
Q18 1 0.9120 0.5553 0.5718 11.00000 0.05 0.22
Q19 1 0.7784 0.4175 0.6294 11.00000 0.05 0.22
Q20 1 0.8863 0.4455 0.6253 11.00000 0.05 0.22
;
_shelx_res_checksum 32309
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN micromount using oil'
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_kjf082q_a
_database_code_depnum_ccdc_archive 'CCDC 1841034'
_audit_update_record
;
2018-05-02 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;
_audit_creation_date 2018-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic
Tris[5-(pentafluorophenyl)dipyrrin]indium(III)
_chemical_formula_moiety 'C45 H18 F15 In N6'
_chemical_formula_sum 'C45 H18 F15 In N6'
_chemical_formula_weight 1042.47
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 10.5034(8)
_cell_length_b 13.5594(11)
_cell_length_c 28.179(2)
_cell_angle_alpha 90
_cell_angle_beta 93.7280(10)
_cell_angle_gamma 90
_cell_volume 4004.7(5)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9920
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 25.36
_cell_measurement_theta_min 2.52
_shelx_estimated_absorpt_T_max 0.933
_shelx_estimated_absorpt_T_min 0.796
_exptl_absorpt_coefficient_mu 0.704
_exptl_absorpt_correction_T_max 0.7452
_exptl_absorpt_correction_T_min 0.6796
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0354 before and 0.0289 after correction. The Ratio of minimum to maximum transmission is 0.9120. The \l/2 correction factor is 0.00150.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light orange'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.729
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2056
_exptl_crystal_preparation ?
_exptl_crystal_recrystallization_method
'The material was recrystallised from DCM by slow evaporation'
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0162
_diffrn_reflns_av_unetI/netI 0.0096
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_number 49555
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 25.376
_diffrn_reflns_theta_max 25.376
_diffrn_reflns_theta_min 1.448
_diffrn_ambient_temperature 100.04
_diffrn_detector 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'Kappa diffractometer'
_diffrn_measurement_device_type 'Bruker APEX2 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'standard sealed X-ray tube'
_diffrn_source_target Mo
_diffrn_source_type 'Siemens, KFF Mo 2K -90 C'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7008
_reflns_number_total 7365
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection 'APEX 3 (Bruker, 2016) '
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XT (Sheldrick, 2015)'
_refine_diff_density_max 0.311
_refine_diff_density_min -0.339
_refine_diff_density_rms 0.048
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.092
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 604
_refine_ls_number_reflns 7365
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0220
_refine_ls_R_factor_gt 0.0204
_refine_ls_restrained_S_all 1.092
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+4.2698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0460
_refine_ls_wR_factor_ref 0.0469
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C1A(H1A), C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C7A(H7A), C1B(H1B),
C2B(H2B), C3B(H3B), C5B(H5B), C6B(H6B), C7B(H7B), C1C(H1C), C2C(H2C), C3C(H3C),
C5C(H5C), C6C(H6C), C7C(H7C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.66830(2) 0.45928(2) 0.63795(2) 0.01264(4) Uani 1 1 d . . . . .
C1A C 1.02278(17) 0.60558(13) 0.69268(6) 0.0201(4) Uani 1 1 d . . . . .
H1A H 1.1020 0.6079 0.7110 0.024 Uiso 1 1 calc R . . . .
C2A C 0.97654(17) 0.67564(13) 0.66039(6) 0.0212(4) Uani 1 1 d . . . . .
H2A H 1.0172 0.7353 0.6523 0.025 Uiso 1 1 calc R . . . .
C3A C 0.85747(17) 0.64108(12) 0.64190(6) 0.0174(3) Uani 1 1 d . . . . .
H3A H 0.8043 0.6746 0.6186 0.021 Uiso 1 1 calc R . . . .
C5A C 0.66721(16) 0.29014(13) 0.71783(6) 0.0177(3) Uani 1 1 d . . . . .
H5A H 0.5834 0.2708 0.7070 0.021 Uiso 1 1 calc R . . . .
C6A C 0.74557(17) 0.23609(13) 0.75156(6) 0.0195(4) Uani 1 1 d . . . . .
H6A H 0.7243 0.1763 0.7668 0.023 Uiso 1 1 calc R . . . .
C7A C 0.85697(17) 0.28686(13) 0.75771(6) 0.0181(4) Uani 1 1 d . . . . .
H7A H 0.9287 0.2692 0.7782 0.022 Uiso 1 1 calc R . . . .
C8A C 0.93708(15) 0.44427(12) 0.72217(6) 0.0149(3) Uani 1 1 d . . . . .
C9A C 0.93032(15) 0.52983(12) 0.69346(6) 0.0151(3) Uani 1 1 d . . . . .
C10A C 0.84638(15) 0.37226(12) 0.72748(6) 0.0147(3) Uani 1 1 d . . . . .
C11A C 1.06224(16) 0.43092(13) 0.75040(6) 0.0166(3) Uani 1 1 d . . . . .
C12A C 1.15579(17) 0.36937(13) 0.73449(6) 0.0199(4) Uani 1 1 d . . . . .
C13A C 1.27388(17) 0.35987(14) 0.75873(7) 0.0228(4) Uani 1 1 d . . . . .
C14A C 1.30094(17) 0.41354(14) 0.79950(7) 0.0236(4) Uani 1 1 d . . . . .
C15A C 1.20966(18) 0.47469(14) 0.81655(7) 0.0256(4) Uani 1 1 d . . . . .
C16A C 1.09173(17) 0.48205(14) 0.79202(7) 0.0223(4) Uani 1 1 d . . . . .
F1A F 1.13279(11) 0.31761(9) 0.69428(4) 0.0321(3) Uani 1 1 d . . . . .
F2A F 1.36183(11) 0.29880(10) 0.74259(4) 0.0372(3) Uani 1 1 d . . . . .
F3A F 1.41654(10) 0.40765(9) 0.82271(4) 0.0348(3) Uani 1 1 d . . . . .
F4A F 1.23727(12) 0.52727(10) 0.85606(5) 0.0435(3) Uani 1 1 d . . . . .
F5A F 1.00427(11) 0.54214(9) 0.80933(4) 0.0370(3) Uani 1 1 d . . . . .
N1A N 0.82859(13) 0.55420(10) 0.66155(5) 0.0145(3) Uani 1 1 d . . . . .
N2A N 0.72486(13) 0.37093(10) 0.70324(5) 0.0148(3) Uani 1 1 d . . . . .
C1B C 0.44494(16) 0.18767(13) 0.60629(6) 0.0176(3) Uani 1 1 d . . . . .
H1B H 0.4371 0.1195 0.5988 0.021 Uiso 1 1 calc R . . . .
C2B C 0.34981(16) 0.24832(13) 0.62015(6) 0.0185(4) Uani 1 1 d . . . . .
H2B H 0.2635 0.2307 0.6239 0.022 Uiso 1 1 calc R . . . .
C3B C 0.40538(16) 0.34211(13) 0.62766(6) 0.0165(3) Uani 1 1 d . . . . .
H3B H 0.3608 0.3984 0.6380 0.020 Uiso 1 1 calc R . . . .
C5B C 0.92381(16) 0.39031(13) 0.59042(6) 0.0185(4) Uani 1 1 d . . . . .
H5B H 0.9589 0.4546 0.5942 0.022 Uiso 1 1 calc R . . . .
C6B C 0.99247(16) 0.30742(14) 0.57554(6) 0.0210(4) Uani 1 1 d . . . . .
H6B H 1.0787 0.3062 0.5672 0.025 Uiso 1 1 calc R . . . .
C7B C 0.91010(16) 0.22928(14) 0.57547(6) 0.0201(4) Uani 1 1 d . . . . .
H7B H 0.9287 0.1630 0.5675 0.024 Uiso 1 1 calc R . . . .
C8B C 0.67839(16) 0.21251(12) 0.59354(6) 0.0155(3) Uani 1 1 d . . . . .
C9B C 0.55787(16) 0.24566(12) 0.60514(6) 0.0152(3) Uani 1 1 d . . . . .
C10B C 0.79069(16) 0.26615(12) 0.58968(6) 0.0157(3) Uani 1 1 d . . . . .
C11B C 0.68858(16) 0.10357(13) 0.58477(6) 0.0170(3) Uani 1 1 d . . . . .
C12B C 0.65915(17) 0.06269(13) 0.54052(6) 0.0197(4) Uani 1 1 d . . . . .
C13B C 0.66788(18) -0.03737(14) 0.53204(7) 0.0232(4) Uani 1 1 d . . . . .
C14B C 0.70556(18) -0.09957(13) 0.56903(7) 0.0235(4) Uani 1 1 d . . . . .
C15B C 0.73748(19) -0.06125(14) 0.61347(7) 0.0248(4) Uani 1 1 d . . . . .
C16B C 0.72899(18) 0.03924(13) 0.62089(6) 0.0217(4) Uani 1 1 d . . . . .
F1B F 0.62061(11) 0.12185(8) 0.50401(4) 0.0285(2) Uani 1 1 d . . . . .
F2B F 0.64021(12) -0.07380(9) 0.48849(4) 0.0357(3) Uani 1 1 d . . . . .
F3B F 0.71239(11) -0.19691(8) 0.56155(4) 0.0331(3) Uani 1 1 d . . . . .
F4B F 0.77628(13) -0.12165(9) 0.64927(4) 0.0405(3) Uani 1 1 d . . . . .
F5B F 0.76128(12) 0.07439(8) 0.66454(4) 0.0317(3) Uani 1 1 d . . . . .
N1B N 0.52913(13) 0.34195(10) 0.61844(5) 0.0147(3) Uani 1 1 d . . . . .
N2B N 0.80368(13) 0.36717(10) 0.59858(5) 0.0153(3) Uani 1 1 d . . . . .
C1C C 0.34751(16) 0.64198(13) 0.68409(6) 0.0185(4) Uani 1 1 d . . . . .
H1C H 0.2745 0.6827 0.6785 0.022 Uiso 1 1 calc R . . . .
C2C C 0.39566(17) 0.60688(13) 0.72757(6) 0.0200(4) Uani 1 1 d . . . . .
H2C H 0.3629 0.6191 0.7577 0.024 Uiso 1 1 calc R . . . .
C3C C 0.50283(16) 0.54938(13) 0.71847(6) 0.0177(3) Uani 1 1 d . . . . .
H3C H 0.5541 0.5154 0.7422 0.021 Uiso 1 1 calc R . . . .
C5C C 0.67217(16) 0.55212(12) 0.53358(6) 0.0170(3) Uani 1 1 d . . . . .
H5C H 0.7509 0.5200 0.5292 0.020 Uiso 1 1 calc R . . . .
C6C C 0.60208(17) 0.60615(13) 0.49761(6) 0.0191(4) Uani 1 1 d . . . . .
H6C H 0.6254 0.6176 0.4661 0.023 Uiso 1 1 calc R . . . .
C7C C 0.49443(17) 0.63849(13) 0.51737(6) 0.0180(4) Uani 1 1 d . . . . .
H7C H 0.4274 0.6759 0.5019 0.022 Uiso 1 1 calc R . . . .
C8C C 0.41700(16) 0.62732(12) 0.60019(6) 0.0158(3) Uani 1 1 d . . . . .
C9C C 0.42756(15) 0.60588(12) 0.64931(6) 0.0151(3) Uani 1 1 d . . . . .
C10C C 0.50140(16) 0.60547(12) 0.56589(6) 0.0155(3) Uani 1 1 d . . . . .
C11C C 0.29727(16) 0.68048(13) 0.58258(6) 0.0177(4) Uani 1 1 d . . . . .
C12C C 0.28797(17) 0.78203(14) 0.58100(6) 0.0224(4) Uani 1 1 d . . . . .
C13C C 0.17816(19) 0.82929(15) 0.56285(7) 0.0274(4) Uani 1 1 d . . . . .
C14C C 0.07447(17) 0.77390(16) 0.54637(7) 0.0273(4) Uani 1 1 d . . . . .
C15C C 0.07983(17) 0.67268(16) 0.54782(7) 0.0253(4) Uani 1 1 d . . . . .
C16C C 0.19056(17) 0.62739(14) 0.56582(6) 0.0213(4) Uani 1 1 d . . . . .
F1C F 0.38814(11) 0.83765(8) 0.59672(4) 0.0292(3) Uani 1 1 d . . . . .
F2C F 0.17274(13) 0.92771(9) 0.56028(5) 0.0411(3) Uani 1 1 d . . . . .
F3C F -0.03199(11) 0.81960(10) 0.52901(4) 0.0396(3) Uani 1 1 d . . . . .
F4C F -0.02142(10) 0.61861(10) 0.53253(4) 0.0358(3) Uani 1 1 d . . . . .
F5C F 0.19324(10) 0.52801(8) 0.56705(4) 0.0283(2) Uani 1 1 d . . . . .
N1C N 0.52327(13) 0.54862(10) 0.67196(5) 0.0153(3) Uani 1 1 d . . . . .
N2C N 0.61459(13) 0.55163(10) 0.57431(5) 0.0147(3) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
In1 0.01242(6) 0.01215(6) 0.01331(6) 0.00053(4) 0.00057(4) 0.00068(4)
C1A 0.0170(8) 0.0213(9) 0.0220(9) 0.0000(7) 0.0004(7) -0.0032(7)
C2A 0.0228(9) 0.0171(9) 0.0238(9) 0.0017(7) 0.0021(7) -0.0058(7)
C3A 0.0223(9) 0.0142(8) 0.0157(8) 0.0007(7) 0.0014(7) 0.0007(7)
C5A 0.0166(8) 0.0199(9) 0.0169(8) 0.0007(7) 0.0030(7) -0.0020(7)
C6A 0.0237(9) 0.0172(9) 0.0179(8) 0.0044(7) 0.0036(7) -0.0006(7)
C7A 0.0196(9) 0.0192(9) 0.0156(8) 0.0029(7) 0.0011(7) 0.0032(7)
C8A 0.0138(8) 0.0165(8) 0.0145(8) -0.0025(6) 0.0021(6) 0.0031(7)
C9A 0.0142(8) 0.0157(8) 0.0156(8) -0.0016(6) 0.0016(6) 0.0006(6)
C10A 0.0146(8) 0.0160(8) 0.0137(8) -0.0007(6) 0.0013(6) 0.0021(7)
C11A 0.0141(8) 0.0170(8) 0.0187(8) 0.0045(7) 0.0008(7) 0.0005(7)
C12A 0.0202(9) 0.0215(9) 0.0181(9) 0.0014(7) 0.0030(7) 0.0023(7)
C13A 0.0165(9) 0.0251(10) 0.0274(10) 0.0085(8) 0.0063(7) 0.0080(7)
C14A 0.0152(9) 0.0228(9) 0.0319(10) 0.0093(8) -0.0064(7) 0.0001(7)
C15A 0.0255(10) 0.0221(10) 0.0278(10) -0.0024(8) -0.0087(8) 0.0012(8)
C16A 0.0194(9) 0.0210(9) 0.0262(10) -0.0028(7) -0.0016(7) 0.0056(7)
F1A 0.0300(6) 0.0431(7) 0.0228(6) -0.0100(5) 0.0000(5) 0.0157(5)
F2A 0.0239(6) 0.0516(8) 0.0362(7) 0.0005(6) 0.0037(5) 0.0219(6)
F3A 0.0196(6) 0.0344(7) 0.0484(7) 0.0062(6) -0.0138(5) 0.0054(5)
F4A 0.0399(7) 0.0415(7) 0.0455(8) -0.0203(6) -0.0255(6) 0.0143(6)
F5A 0.0296(6) 0.0451(7) 0.0345(7) -0.0213(6) -0.0114(5) 0.0196(6)
N1A 0.0157(7) 0.0130(7) 0.0147(7) -0.0005(5) 0.0007(5) 0.0003(6)
N2A 0.0133(7) 0.0163(7) 0.0149(7) 0.0006(6) 0.0013(5) 0.0002(6)
C1B 0.0204(9) 0.0165(9) 0.0156(8) 0.0005(7) -0.0004(7) -0.0025(7)
C2B 0.0149(8) 0.0218(9) 0.0187(8) 0.0021(7) 0.0009(7) -0.0033(7)
C3B 0.0152(8) 0.0187(9) 0.0154(8) 0.0008(7) 0.0006(6) 0.0020(7)
C5B 0.0173(8) 0.0202(9) 0.0182(8) 0.0010(7) 0.0020(7) -0.0009(7)
C6B 0.0139(8) 0.0265(10) 0.0228(9) 0.0012(7) 0.0037(7) 0.0030(7)
C7B 0.0189(9) 0.0199(9) 0.0215(9) -0.0004(7) 0.0024(7) 0.0055(7)
C8B 0.0193(8) 0.0152(8) 0.0117(8) 0.0006(6) -0.0003(6) 0.0010(7)
C9B 0.0178(8) 0.0143(8) 0.0133(8) 0.0008(6) -0.0004(6) 0.0000(7)
C10B 0.0175(8) 0.0153(8) 0.0143(8) 0.0008(6) 0.0002(6) 0.0024(7)
C11B 0.0146(8) 0.0159(9) 0.0208(9) -0.0003(7) 0.0030(7) 0.0006(7)
C12B 0.0199(9) 0.0181(9) 0.0209(9) 0.0025(7) -0.0002(7) 0.0017(7)
C13B 0.0241(9) 0.0217(9) 0.0235(9) -0.0069(8) -0.0003(7) -0.0022(8)
C14B 0.0238(9) 0.0129(9) 0.0341(11) -0.0019(8) 0.0047(8) 0.0005(7)
C15B 0.0294(10) 0.0178(9) 0.0271(10) 0.0061(8) 0.0013(8) 0.0040(8)
C16B 0.0259(9) 0.0200(9) 0.0190(9) -0.0007(7) 0.0012(7) 0.0017(8)
F1B 0.0428(7) 0.0228(6) 0.0189(5) 0.0017(4) -0.0058(5) 0.0043(5)
F2B 0.0503(8) 0.0279(6) 0.0278(6) -0.0128(5) -0.0068(5) -0.0004(5)
F3B 0.0404(7) 0.0127(5) 0.0463(7) -0.0044(5) 0.0025(6) 0.0005(5)
F4B 0.0651(9) 0.0217(6) 0.0339(7) 0.0101(5) -0.0037(6) 0.0102(6)
F5B 0.0507(7) 0.0249(6) 0.0185(5) -0.0011(5) -0.0058(5) 0.0062(5)
N1B 0.0144(7) 0.0153(7) 0.0142(7) 0.0004(5) 0.0007(5) 0.0005(6)
N2B 0.0154(7) 0.0146(7) 0.0160(7) 0.0003(6) 0.0020(5) 0.0003(6)
C1C 0.0156(8) 0.0170(9) 0.0233(9) -0.0012(7) 0.0038(7) 0.0007(7)
C2C 0.0214(9) 0.0205(9) 0.0188(9) -0.0020(7) 0.0066(7) -0.0009(7)
C3C 0.0208(9) 0.0166(8) 0.0155(8) 0.0005(7) 0.0005(7) -0.0012(7)
C5C 0.0163(8) 0.0171(8) 0.0178(8) -0.0005(7) 0.0024(7) -0.0012(7)
C6C 0.0228(9) 0.0203(9) 0.0141(8) 0.0024(7) 0.0024(7) -0.0021(7)
C7C 0.0203(9) 0.0157(8) 0.0175(8) 0.0021(7) -0.0021(7) 0.0010(7)
C8C 0.0151(8) 0.0125(8) 0.0197(9) -0.0006(7) -0.0007(7) -0.0012(6)
C9C 0.0132(8) 0.0127(8) 0.0195(8) -0.0003(6) 0.0015(6) -0.0009(6)
C10C 0.0154(8) 0.0132(8) 0.0176(8) 0.0003(6) -0.0007(6) -0.0007(6)
C11C 0.0160(8) 0.0221(9) 0.0152(8) 0.0017(7) 0.0027(7) 0.0048(7)
C12C 0.0226(9) 0.0230(9) 0.0216(9) -0.0014(7) 0.0008(7) 0.0041(8)
C13C 0.0322(11) 0.0245(10) 0.0257(10) 0.0025(8) 0.0037(8) 0.0141(8)
C14C 0.0176(9) 0.0439(12) 0.0204(9) 0.0054(8) 0.0019(7) 0.0147(9)
C15C 0.0147(9) 0.0413(12) 0.0199(9) 0.0037(8) 0.0013(7) 0.0001(8)
C16C 0.0191(9) 0.0251(10) 0.0202(9) 0.0025(7) 0.0035(7) 0.0004(7)
F1C 0.0319(6) 0.0187(5) 0.0359(6) -0.0022(5) -0.0072(5) 0.0024(5)
F2C 0.0481(8) 0.0260(6) 0.0481(8) 0.0001(6) -0.0055(6) 0.0201(6)
F3C 0.0239(6) 0.0586(8) 0.0360(7) 0.0076(6) -0.0009(5) 0.0225(6)
F4C 0.0163(5) 0.0562(8) 0.0340(6) 0.0085(6) -0.0052(5) -0.0067(5)
F5C 0.0234(6) 0.0245(6) 0.0364(6) 0.0028(5) -0.0022(5) -0.0049(5)
N1C 0.0157(7) 0.0146(7) 0.0157(7) -0.0001(6) 0.0006(5) 0.0005(6)
N2C 0.0146(7) 0.0145(7) 0.0149(7) 0.0007(5) 0.0006(5) 0.0006(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
In1 N1A 2.1880(14) . ?
In1 N2A 2.2429(14) . ?
In1 N1B 2.2059(14) . ?
In1 N2B 2.2402(14) . ?
In1 N1C 2.2127(14) . ?
In1 N2C 2.2296(14) . ?
C1A H1A 0.9500 . ?
C1A C2A 1.382(3) . ?
C1A C9A 1.415(2) . ?
C2A H2A 0.9500 . ?
C2A C3A 1.404(2) . ?
C3A H3A 0.9500 . ?
C3A N1A 1.345(2) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.420(2) . ?
C5A N2A 1.330(2) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.359(3) . ?
C7A H7A 0.9500 . ?
C7A C10A 1.438(2) . ?
C8A C9A 1.414(2) . ?
C8A C10A 1.379(2) . ?
C8A C11A 1.503(2) . ?
C9A N1A 1.391(2) . ?
C10A N2A 1.408(2) . ?
C11A C12A 1.386(2) . ?
C11A C16A 1.380(3) . ?
C12A C13A 1.383(3) . ?
C12A F1A 1.341(2) . ?
C13A C14A 1.374(3) . ?
C13A F2A 1.342(2) . ?
C14A C15A 1.378(3) . ?
C14A F3A 1.344(2) . ?
C15A C16A 1.382(3) . ?
C15A F4A 1.338(2) . ?
C16A F5A 1.343(2) . ?
C1B H1B 0.9500 . ?
C1B C2B 1.370(2) . ?
C1B C9B 1.425(2) . ?
C2B H2B 0.9500 . ?
C2B C3B 1.410(2) . ?
C3B H3B 0.9500 . ?
C3B N1B 1.342(2) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.414(3) . ?
C5B N2B 1.335(2) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.368(3) . ?
C7B H7B 0.9500 . ?
C7B C10B 1.431(2) . ?
C8B C9B 1.402(2) . ?
C8B C10B 1.396(2) . ?
C8B C11B 1.503(2) . ?
C9B N1B 1.397(2) . ?
C10B N2B 1.398(2) . ?
C11B C12B 1.381(2) . ?
C11B C16B 1.386(2) . ?
C12B C13B 1.382(3) . ?
C12B F1B 1.346(2) . ?
C13B C14B 1.379(3) . ?
C13B F2B 1.337(2) . ?
C14B C15B 1.377(3) . ?
C14B F3B 1.339(2) . ?
C15B C16B 1.382(3) . ?
C15B F4B 1.342(2) . ?
C16B F5B 1.342(2) . ?
C1C H1C 0.9500 . ?
C1C C2C 1.380(3) . ?
C1C C9C 1.419(2) . ?
C2C H2C 0.9500 . ?
C2C C3C 1.407(2) . ?
C3C H3C 0.9500 . ?
C3C N1C 1.342(2) . ?
C5C H5C 0.9500 . ?
C5C C6C 1.417(2) . ?
C5C N2C 1.332(2) . ?
C6C H6C 0.9500 . ?
C6C C7C 1.365(2) . ?
C7C H7C 0.9500 . ?
C7C C10C 1.436(2) . ?
C8C C9C 1.412(2) . ?
C8C C10C 1.385(2) . ?
C8C C11C 1.505(2) . ?
C9C N1C 1.392(2) . ?
C10C N2C 1.402(2) . ?
C11C C12C 1.381(3) . ?
C11C C16C 1.389(3) . ?
C12C C13C 1.388(3) . ?
C12C F1C 1.346(2) . ?
C13C C14C 1.379(3) . ?
C13C F2C 1.337(2) . ?
C14C C15C 1.374(3) . ?
C14C F3C 1.342(2) . ?
C15C C16C 1.382(3) . ?
C15C F4C 1.340(2) . ?
C16C F5C 1.348(2) . ?
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
N1A In1 N2A 84.69(5) . . ?
N1A In1 N1B 169.85(5) . . ?
N1A In1 N2B 88.73(5) . . ?
N1A In1 N1C 94.83(5) . . ?
N1A In1 N2C 93.64(5) . . ?
N1B In1 N2A 87.43(5) . . ?
N1B In1 N2B 84.61(5) . . ?
N1B In1 N1C 92.24(5) . . ?
N1B In1 N2C 94.34(5) . . ?
N2B In1 N2A 88.03(5) . . ?
N1C In1 N2A 95.18(5) . . ?
N1C In1 N2B 175.41(5) . . ?
N1C In1 N2C 84.01(5) . . ?
N2C In1 N2A 178.08(5) . . ?
N2C In1 N2B 92.88(5) . . ?
C2A C1A H1A 126.4 . . ?
C2A C1A C9A 107.28(15) . . ?
C9A C1A H1A 126.4 . . ?
C1A C2A H2A 126.8 . . ?
C1A C2A C3A 106.35(16) . . ?
C3A C2A H2A 126.8 . . ?
C2A C3A H3A 124.5 . . ?
N1A C3A C2A 111.04(15) . . ?
N1A C3A H3A 124.5 . . ?
C6A C5A H5A 123.9 . . ?
N2A C5A H5A 123.9 . . ?
N2A C5A C6A 112.11(15) . . ?
C5A C6A H6A 126.8 . . ?
C7A C6A C5A 106.31(15) . . ?
C7A C6A H6A 126.8 . . ?
C6A C7A H7A 126.3 . . ?
C6A C7A C10A 107.43(15) . . ?
C10A C7A H7A 126.3 . . ?
C9A C8A C11A 114.30(15) . . ?
C10A C8A C9A 129.34(15) . . ?
C10A C8A C11A 116.36(15) . . ?
C8A C9A C1A 126.57(16) . . ?
N1A C9A C1A 108.47(15) . . ?
N1A C9A C8A 124.95(15) . . ?
C8A C10A C7A 127.39(15) . . ?
C8A C10A N2A 124.56(15) . . ?
N2A C10A C7A 108.05(14) . . ?
C12A C11A C8A 121.05(15) . . ?
C16A C11A C8A 121.98(15) . . ?
C16A C11A C12A 116.92(16) . . ?
C13A C12A C11A 121.91(17) . . ?
F1A C12A C11A 119.72(15) . . ?
F1A C12A C13A 118.37(16) . . ?
C14A C13A C12A 119.60(17) . . ?
F2A C13A C12A 120.34(17) . . ?
F2A C13A C14A 120.05(16) . . ?
C13A C14A C15A 119.97(16) . . ?
F3A C14A C13A 120.46(17) . . ?
F3A C14A C15A 119.57(17) . . ?
C14A C15A C16A 119.37(17) . . ?
F4A C15A C14A 119.53(17) . . ?
F4A C15A C16A 121.09(17) . . ?
C11A C16A C15A 122.20(17) . . ?
F5A C16A C11A 119.50(16) . . ?
F5A C16A C15A 118.29(17) . . ?
C3A N1A In1 125.45(11) . . ?
C3A N1A C9A 106.85(14) . . ?
C9A N1A In1 126.89(11) . . ?
C5A N2A In1 126.30(11) . . ?
C5A N2A C10A 106.10(14) . . ?
C10A N2A In1 125.06(11) . . ?
C2B C1B H1B 126.3 . . ?
C2B C1B C9B 107.38(15) . . ?
C9B C1B H1B 126.3 . . ?
C1B C2B H2B 126.8 . . ?
C1B C2B C3B 106.37(15) . . ?
C3B C2B H2B 126.8 . . ?
C2B C3B H3B 124.3 . . ?
N1B C3B C2B 111.49(15) . . ?
N1B C3B H3B 124.3 . . ?
C6B C5B H5B 124.1 . . ?
N2B C5B H5B 124.1 . . ?
N2B C5B C6B 111.74(16) . . ?
C5B C6B H6B 126.8 . . ?
C7B C6B C5B 106.35(15) . . ?
C7B C6B H6B 126.8 . . ?
C6B C7B H7B 126.4 . . ?
C6B C7B C10B 107.14(16) . . ?
C10B C7B H7B 126.4 . . ?
C9B C8B C11B 115.38(15) . . ?
C10B C8B C9B 129.16(16) . . ?
C10B C8B C11B 115.45(15) . . ?
C8B C9B C1B 126.43(16) . . ?
N1B C9B C1B 108.36(14) . . ?
N1B C9B C8B 125.20(15) . . ?
C8B C10B C7B 126.87(16) . . ?
C8B C10B N2B 124.73(15) . . ?
N2B C10B C7B 108.38(15) . . ?
C12B C11B C8B 121.93(15) . . ?
C12B C11B C16B 116.76(16) . . ?
C16B C11B C8B 121.31(16) . . ?
C11B C12B C13B 122.46(17) . . ?
F1B C12B C11B 119.31(16) . . ?
F1B C12B C13B 118.23(16) . . ?
C14B C13B C12B 119.27(17) . . ?
F2B C13B C12B 120.56(17) . . ?
F2B C13B C14B 120.16(17) . . ?
C15B C14B C13B 119.85(17) . . ?
F3B C14B C13B 119.96(17) . . ?
F3B C14B C15B 120.18(17) . . ?
C14B C15B C16B 119.68(17) . . ?
F4B C15B C14B 119.82(17) . . ?
F4B C15B C16B 120.50(17) . . ?
C15B C16B C11B 121.95(17) . . ?
F5B C16B C11B 119.78(16) . . ?
F5B C16B C15B 118.27(16) . . ?
C3B N1B In1 125.81(11) . . ?
C3B N1B C9B 106.40(14) . . ?
C9B N1B In1 126.14(11) . . ?
C5B N2B In1 126.29(12) . . ?
C5B N2B C10B 106.38(14) . . ?
C10B N2B In1 125.28(11) . . ?
C2C C1C H1C 126.4 . . ?
C2C C1C C9C 107.15(15) . . ?
C9C C1C H1C 126.4 . . ?
C1C C2C H2C 126.8 . . ?
C1C C2C C3C 106.31(15) . . ?
C3C C2C H2C 126.8 . . ?
C2C C3C H3C 124.4 . . ?
N1C C3C C2C 111.29(15) . . ?
N1C C3C H3C 124.4 . . ?
C6C C5C H5C 124.0 . . ?
N2C C5C H5C 124.0 . . ?
N2C C5C C6C 112.02(15) . . ?
C5C C6C H6C 126.9 . . ?
C7C C6C C5C 106.25(15) . . ?
C7C C6C H6C 126.9 . . ?
C6C C7C H7C 126.4 . . ?
C6C C7C C10C 107.21(15) . . ?
C10C C7C H7C 126.4 . . ?
C9C C8C C11C 115.63(15) . . ?
C10C C8C C9C 128.83(16) . . ?
C10C C8C C11C 115.54(15) . . ?
C8C C9C C1C 126.42(16) . . ?
N1C C9C C1C 108.57(15) . . ?
N1C C9C C8C 124.95(15) . . ?
C8C C10C C7C 127.03(16) . . ?
C8C C10C N2C 124.57(15) . . ?
N2C C10C C7C 108.27(14) . . ?
C12C C11C C8C 122.95(16) . . ?
C12C C11C C16C 116.87(16) . . ?
C16C C11C C8C 120.16(16) . . ?
C11C C12C C13C 121.85(18) . . ?
F1C C12C C11C 119.73(16) . . ?
F1C C12C C13C 118.41(17) . . ?
C14C C13C C12C 119.48(18) . . ?
F2C C13C C12C 120.80(19) . . ?
F2C C13C C14C 119.70(17) . . ?
C15C C14C C13C 120.28(17) . . ?
F3C C14C C13C 119.49(19) . . ?
F3C C14C C15C 120.23(19) . . ?
C14C C15C C16C 119.12(18) . . ?
F4C C15C C14C 120.46(17) . . ?
F4C C15C C16C 120.42(18) . . ?
C15C C16C C11C 122.39(18) . . ?
F5C C16C C11C 119.62(16) . . ?
F5C C16C C15C 117.99(17) . . ?
C3C N1C In1 125.85(11) . . ?
C3C N1C C9C 106.68(14) . . ?
C9C N1C In1 127.14(11) . . ?
C5C N2C In1 126.21(11) . . ?
C5C N2C C10C 106.22(14) . . ?
C10C N2C In1 126.58(11) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2A H2A F3A 0.95 2.53 3.364(2) 147.3 2_756
C3A H3A F3B 0.95 2.52 3.439(2) 162.9 1_565
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
C1A C2A C3A N1A 0.5(2) . . . . ?
C1A C9A N1A In1 170.25(11) . . . . ?
C1A C9A N1A C3A 0.16(18) . . . . ?
C2A C1A C9A C8A -178.72(16) . . . . ?
C2A C1A C9A N1A 0.1(2) . . . . ?
C2A C3A N1A In1 -170.68(11) . . . . ?
C2A C3A N1A C9A -0.41(19) . . . . ?
C5A C6A C7A C10A -0.09(19) . . . . ?
C6A C5A N2A In1 162.73(11) . . . . ?
C6A C5A N2A C10A 0.21(19) . . . . ?
C6A C7A C10A C8A -179.73(17) . . . . ?
C6A C7A C10A N2A 0.22(19) . . . . ?
C7A C10A N2A In1 -163.05(11) . . . . ?
C7A C10A N2A C5A -0.26(18) . . . . ?
C8A C9A N1A In1 -10.9(2) . . . . ?
C8A C9A N1A C3A 179.04(16) . . . . ?
C8A C10A N2A In1 16.9(2) . . . . ?
C8A C10A N2A C5A 179.69(16) . . . . ?
C8A C11A C12A C13A 176.74(16) . . . . ?
C8A C11A C12A F1A -2.8(3) . . . . ?
C8A C11A C16A C15A -175.88(17) . . . . ?
C8A C11A C16A F5A 3.3(3) . . . . ?
C9A C1A C2A C3A -0.4(2) . . . . ?
C9A C8A C10A C7A -179.10(17) . . . . ?
C9A C8A C10A N2A 1.0(3) . . . . ?
C9A C8A C11A C12A -97.89(19) . . . . ?
C9A C8A C11A C16A 79.3(2) . . . . ?
C10A C8A C9A C1A 174.04(17) . . . . ?
C10A C8A C9A N1A -4.6(3) . . . . ?
C10A C8A C11A C12A 81.7(2) . . . . ?
C10A C8A C11A C16A -101.1(2) . . . . ?
C11A C8A C9A C1A -6.4(2) . . . . ?
C11A C8A C9A N1A 174.88(15) . . . . ?
C11A C8A C10A C7A 1.4(3) . . . . ?
C11A C8A C10A N2A -178.54(15) . . . . ?
C11A C12A C13A C14A -0.8(3) . . . . ?
C11A C12A C13A F2A 179.31(16) . . . . ?
C12A C11A C16A C15A 1.4(3) . . . . ?
C12A C11A C16A F5A -179.42(16) . . . . ?
C12A C13A C14A C15A 1.4(3) . . . . ?
C12A C13A C14A F3A -177.88(16) . . . . ?
C13A C14A C15A C16A -0.6(3) . . . . ?
C13A C14A C15A F4A -179.46(18) . . . . ?
C14A C15A C16A C11A -0.8(3) . . . . ?
C14A C15A C16A F5A 180.00(18) . . . . ?
C16A C11A C12A C13A -0.6(3) . . . . ?
C16A C11A C12A F1A 179.92(16) . . . . ?
F1A C12A C13A C14A 178.68(16) . . . . ?
F1A C12A C13A F2A -1.2(3) . . . . ?
F2A C13A C14A C15A -178.70(17) . . . . ?
F2A C13A C14A F3A 2.0(3) . . . . ?
F3A C14A C15A C16A 178.68(17) . . . . ?
F3A C14A C15A F4A -0.1(3) . . . . ?
F4A C15A C16A C11A 177.98(18) . . . . ?
F4A C15A C16A F5A -1.2(3) . . . . ?
N2A C5A C6A C7A -0.1(2) . . . . ?
C1B C2B C3B N1B 0.8(2) . . . . ?
C1B C9B N1B In1 166.58(11) . . . . ?
C1B C9B N1B C3B 0.60(18) . . . . ?
C2B C1B C9B C8B 178.90(16) . . . . ?
C2B C1B C9B N1B -0.09(19) . . . . ?
C2B C3B N1B In1 -166.94(11) . . . . ?
C2B C3B N1B C9B -0.89(18) . . . . ?
C5B C6B C7B C10B 0.9(2) . . . . ?
C6B C5B N2B In1 165.08(11) . . . . ?
C6B C5B N2B C10B 0.78(19) . . . . ?
C6B C7B C10B C8B 178.54(17) . . . . ?
C6B C7B C10B N2B -0.49(19) . . . . ?
C7B C10B N2B In1 -164.68(11) . . . . ?
C7B C10B N2B C5B -0.18(18) . . . . ?
C8B C9B N1B In1 -12.4(2) . . . . ?
C8B C9B N1B C3B -178.41(16) . . . . ?
C8B C10B N2B In1 16.3(2) . . . . ?
C8B C10B N2B C5B -179.23(16) . . . . ?
C8B C11B C12B C13B -179.86(17) . . . . ?
C8B C11B C12B F1B 0.2(3) . . . . ?
C8B C11B C16B C15B 179.27(17) . . . . ?
C8B C11B C16B F5B -0.8(3) . . . . ?
C9B C1B C2B C3B -0.43(19) . . . . ?
C9B C8B C10B C7B -176.79(17) . . . . ?
C9B C8B C10B N2B 2.1(3) . . . . ?
C9B C8B C11B C12B 87.0(2) . . . . ?
C9B C8B C11B C16B -93.4(2) . . . . ?
C10B C8B C9B C1B 176.76(17) . . . . ?
C10B C8B C9B N1B -4.4(3) . . . . ?
C10B C8B C11B C12B -93.9(2) . . . . ?
C10B C8B C11B C16B 85.7(2) . . . . ?
C11B C8B C9B C1B -4.3(2) . . . . ?
C11B C8B C9B N1B 174.53(15) . . . . ?
C11B C8B C10B C7B 4.3(3) . . . . ?
C11B C8B C10B N2B -176.86(15) . . . . ?
C11B C12B C13B C14B 0.9(3) . . . . ?
C11B C12B C13B F2B -179.05(16) . . . . ?
C12B C11B C16B C15B -1.1(3) . . . . ?
C12B C11B C16B F5B 178.81(16) . . . . ?
C12B C13B C14B C15B -1.9(3) . . . . ?
C12B C13B C14B F3B 178.87(17) . . . . ?
C13B C14B C15B C16B 1.3(3) . . . . ?
C13B C14B C15B F4B -178.84(17) . . . . ?
C14B C15B C16B C11B 0.2(3) . . . . ?
C14B C15B C16B F5B -179.72(17) . . . . ?
C16B C11B C12B C13B 0.6(3) . . . . ?
C16B C11B C12B F1B -179.34(16) . . . . ?
F1B C12B C13B C14B -179.17(16) . . . . ?
F1B C12B C13B F2B 0.9(3) . . . . ?
F2B C13B C14B C15B 178.11(17) . . . . ?
F2B C13B C14B F3B -1.1(3) . . . . ?
F3B C14B C15B C16B -179.43(17) . . . . ?
F3B C14B C15B F4B 0.4(3) . . . . ?
F4B C15B C16B C11B -179.62(17) . . . . ?
F4B C15B C16B F5B 0.4(3) . . . . ?
N2B C5B C6B C7B -1.1(2) . . . . ?
C1C C2C C3C N1C 0.7(2) . . . . ?
C1C C9C N1C In1 173.71(11) . . . . ?
C1C C9C N1C C3C 0.09(18) . . . . ?
C2C C1C C9C C8C -176.93(16) . . . . ?
C2C C1C C9C N1C 0.37(19) . . . . ?
C2C C3C N1C In1 -174.24(11) . . . . ?
C2C C3C N1C C9C -0.52(19) . . . . ?
C5C C6C C7C C10C 1.29(19) . . . . ?
C6C C5C N2C In1 169.93(11) . . . . ?
C6C C5C N2C C10C 0.81(19) . . . . ?
C6C C7C C10C C8C 175.13(17) . . . . ?
C6C C7C C10C N2C -0.85(19) . . . . ?
C7C C10C N2C In1 -169.05(11) . . . . ?
C7C C10C N2C C5C 0.02(18) . . . . ?
C8C C9C N1C In1 -8.9(2) . . . . ?
C8C C9C N1C C3C 177.44(16) . . . . ?
C8C C10C N2C In1 14.8(2) . . . . ?
C8C C10C N2C C5C -176.09(16) . . . . ?
C8C C11C C12C C13C 177.39(17) . . . . ?
C8C C11C C12C F1C -1.6(3) . . . . ?
C8C C11C C16C C15C -177.81(16) . . . . ?
C8C C11C C16C F5C 2.4(2) . . . . ?
C9C C1C C2C C3C -0.7(2) . . . . ?
C9C C8C C10C C7C -172.14(17) . . . . ?
C9C C8C C10C N2C 3.2(3) . . . . ?
C9C C8C C11C C12C 90.2(2) . . . . ?
C9C C8C C11C C16C -91.4(2) . . . . ?
C10C C8C C9C C1C 170.35(17) . . . . ?
C10C C8C C9C N1C -6.5(3) . . . . ?
C10C C8C C11C C12C -90.3(2) . . . . ?
C10C C8C C11C C16C 88.1(2) . . . . ?
C11C C8C C9C C1C -10.2(2) . . . . ?
C11C C8C C9C N1C 172.95(15) . . . . ?
C11C C8C C10C C7C 8.4(3) . . . . ?
C11C C8C C10C N2C -176.25(15) . . . . ?
C11C C12C C13C C14C 0.8(3) . . . . ?
C11C C12C C13C F2C -177.85(17) . . . . ?
C12C C11C C16C C15C 0.6(3) . . . . ?
C12C C11C C16C F5C -179.10(16) . . . . ?
C12C C13C C14C C15C -0.1(3) . . . . ?
C12C C13C C14C F3C 179.69(17) . . . . ?
C13C C14C C15C C16C -0.3(3) . . . . ?
C13C C14C C15C F4C 178.94(17) . . . . ?
C14C C15C C16C C11C 0.0(3) . . . . ?
C14C C15C C16C F5C 179.73(16) . . . . ?
C16C C11C C12C C13C -1.0(3) . . . . ?
C16C C11C C12C F1C -179.98(15) . . . . ?
F1C C12C C13C C14C 179.74(16) . . . . ?
F1C C12C C13C F2C 1.1(3) . . . . ?
F2C C13C C14C C15C 178.53(18) . . . . ?
F2C C13C C14C F3C -1.7(3) . . . . ?
F3C C14C C15C C16C 179.95(16) . . . . ?
F3C C14C C15C F4C -0.8(3) . . . . ?
F4C C15C C16C C11C -179.22(16) . . . . ?
F4C C15C C16C F5C 0.5(3) . . . . ?
N2C C5C C6C C7C -1.4(2) . . . . ?
_shelx_res_file
;
kjf082q_a.res created by SHELXL-2014/7
TITL kjf082q_a.res in P2(1)/n
REM Old TITL kjf082q in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.082, Rweak 0.004, Alpha 0.034, Orientation as input
REM Formula found by SHELXT: C45 N6 F15 In
CELL 0.71073 10.5034 13.5594 28.1787 90 93.728 90
ZERR 4 0.0008 0.0011 0.0022 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H F In N
UNIT 180 72 60 4 24
EQIV $1 +X,1+Y,+Z
EQIV $2 2.5-X,0.5+Y,1.5-Z
L.S. 10
PLAN 20
SIZE 0.1 0.11 0.34
TEMP -173.11
HTAB C3A F3B_$1
HTAB C2A F3A_$2
BOND $H
LIST 6
HTAB
MORE -1
CONF
fmap 2
acta 52
REM
REM
REM
WGHT 0.013200 4.269800
FVAR 0.24375
IN1 4 0.668304 0.459285 0.637954 11.00000 0.01242 0.01215 =
0.01331 0.00053 0.00057 0.00068
C1A 1 1.022783 0.605577 0.692681 11.00000 0.01700 0.02125 =
0.02198 0.00001 0.00042 -0.00323
AFIX 43
H1A 2 1.101965 0.607852 0.710970 11.00000 -1.20000
AFIX 0
C2A 1 0.976538 0.675635 0.660385 11.00000 0.02279 0.01706 =
0.02379 0.00172 0.00215 -0.00578
AFIX 43
H2A 2 1.017241 0.735328 0.652297 11.00000 -1.20000
AFIX 0
C3A 1 0.857467 0.641082 0.641901 11.00000 0.02231 0.01418 =
0.01568 0.00066 0.00142 0.00074
AFIX 43
H3A 2 0.804308 0.674640 0.618592 11.00000 -1.20000
AFIX 0
C5A 1 0.667208 0.290143 0.717832 11.00000 0.01657 0.01990 =
0.01688 0.00072 0.00299 -0.00205
AFIX 43
H5A 2 0.583381 0.270841 0.706960 11.00000 -1.20000
AFIX 0
C6A 1 0.745565 0.236093 0.751561 11.00000 0.02369 0.01725 =
0.01790 0.00442 0.00358 -0.00056
AFIX 43
H6A 2 0.724344 0.176349 0.766789 11.00000 -1.20000
AFIX 0
C7A 1 0.856972 0.286863 0.757715 11.00000 0.01958 0.01916 =
0.01565 0.00287 0.00109 0.00322
AFIX 43
H7A 2 0.928686 0.269170 0.778230 11.00000 -1.20000
AFIX 0
C8A 1 0.937077 0.444273 0.722169 11.00000 0.01383 0.01650 =
0.01447 -0.00254 0.00211 0.00307
C9A 1 0.930324 0.529832 0.693456 11.00000 0.01415 0.01567 =
0.01556 -0.00163 0.00162 0.00055
C10A 1 0.846378 0.372264 0.727480 11.00000 0.01458 0.01600 =
0.01371 -0.00071 0.00132 0.00214
C11A 1 1.062243 0.430922 0.750398 11.00000 0.01407 0.01701 =
0.01868 0.00450 0.00077 0.00047
C12A 1 1.155794 0.369366 0.734493 11.00000 0.02019 0.02153 =
0.01811 0.00142 0.00296 0.00232
C13A 1 1.273880 0.359865 0.758735 11.00000 0.01655 0.02509 =
0.02742 0.00851 0.00629 0.00805
C14A 1 1.300945 0.413536 0.799495 11.00000 0.01515 0.02281 =
0.03186 0.00930 -0.00644 0.00008
C15A 1 1.209658 0.474689 0.816546 11.00000 0.02554 0.02209 =
0.02783 -0.00242 -0.00874 0.00125
C16A 1 1.091729 0.482053 0.792019 11.00000 0.01938 0.02104 =
0.02620 -0.00276 -0.00155 0.00565
F1A 3 1.132791 0.317612 0.694285 11.00000 0.03001 0.04309 =
0.02284 -0.00995 -0.00002 0.01571
F2A 3 1.361827 0.298799 0.742588 11.00000 0.02390 0.05159 =
0.03621 0.00049 0.00374 0.02187
F3A 3 1.416544 0.407655 0.822706 11.00000 0.01962 0.03442 =
0.04842 0.00615 -0.01376 0.00541
F4A 3 1.237268 0.527266 0.856058 11.00000 0.03992 0.04153 =
0.04546 -0.02030 -0.02551 0.01429
F5A 3 1.004270 0.542144 0.809335 11.00000 0.02961 0.04508 =
0.03447 -0.02132 -0.01137 0.01956
N1A 5 0.828592 0.554198 0.661547 11.00000 0.01570 0.01301 =
0.01471 -0.00050 0.00074 0.00031
N2A 5 0.724857 0.370930 0.703241 11.00000 0.01333 0.01635 =
0.01485 0.00062 0.00130 0.00025
C1B 1 0.444937 0.187666 0.606287 11.00000 0.02038 0.01649 =
0.01564 0.00054 -0.00044 -0.00250
AFIX 43
H1B 2 0.437058 0.119529 0.598817 11.00000 -1.20000
AFIX 0
C2B 1 0.349814 0.248317 0.620149 11.00000 0.01490 0.02181 =
0.01865 0.00214 0.00094 -0.00331
AFIX 43
H2B 2 0.263543 0.230653 0.623944 11.00000 -1.20000
AFIX 0
C3B 1 0.405381 0.342114 0.627660 11.00000 0.01522 0.01873 =
0.01541 0.00078 0.00063 0.00204
AFIX 43
H3B 2 0.360831 0.398365 0.637953 11.00000 -1.20000
AFIX 0
C5B 1 0.923812 0.390314 0.590420 11.00000 0.01732 0.02016 =
0.01818 0.00098 0.00205 -0.00093
AFIX 43
H5B 2 0.958899 0.454635 0.594155 11.00000 -1.20000
AFIX 0
C6B 1 0.992469 0.307420 0.575541 11.00000 0.01393 0.02654 =
0.02280 0.00122 0.00371 0.00304
AFIX 43
H6B 2 1.078684 0.306224 0.567243 11.00000 -1.20000
AFIX 0
C7B 1 0.910105 0.229281 0.575468 11.00000 0.01890 0.01992 =
0.02155 -0.00036 0.00244 0.00548
AFIX 43
H7B 2 0.928669 0.162982 0.567484 11.00000 -1.20000
AFIX 0
C8B 1 0.678392 0.212508 0.593544 11.00000 0.01934 0.01521 =
0.01169 0.00062 -0.00028 0.00104
C9B 1 0.557872 0.245659 0.605144 11.00000 0.01782 0.01428 =
0.01327 0.00081 -0.00043 0.00002
C10B 1 0.790692 0.266150 0.589678 11.00000 0.01746 0.01532 =
0.01430 0.00078 0.00022 0.00241
C11B 1 0.688579 0.103566 0.584772 11.00000 0.01462 0.01586 =
0.02084 -0.00028 0.00300 0.00059
C12B 1 0.659154 0.062689 0.540521 11.00000 0.01994 0.01811 =
0.02088 0.00248 -0.00017 0.00169
C13B 1 0.667876 -0.037374 0.532042 11.00000 0.02412 0.02173 =
0.02353 -0.00693 -0.00028 -0.00224
C14B 1 0.705556 -0.099574 0.569034 11.00000 0.02375 0.01287 =
0.03415 -0.00192 0.00470 0.00050
C15B 1 0.737479 -0.061253 0.613475 11.00000 0.02936 0.01779 =
0.02714 0.00612 0.00132 0.00398
C16B 1 0.728992 0.039242 0.620888 11.00000 0.02588 0.02000 =
0.01903 -0.00070 0.00121 0.00172
F1B 3 0.620608 0.121847 0.504009 11.00000 0.04279 0.02284 =
0.01892 0.00168 -0.00580 0.00432
F2B 3 0.640210 -0.073803 0.488490 11.00000 0.05025 0.02794 =
0.02776 -0.01279 -0.00676 -0.00037
F3B 3 0.712386 -0.196912 0.561548 11.00000 0.04044 0.01265 =
0.04631 -0.00436 0.00246 0.00050
F4B 3 0.776280 -0.121652 0.649266 11.00000 0.06511 0.02168 =
0.03394 0.01012 -0.00373 0.01022
F5B 3 0.761277 0.074387 0.664540 11.00000 0.05065 0.02492 =
0.01846 -0.00110 -0.00579 0.00617
N1B 5 0.529128 0.341953 0.618441 11.00000 0.01441 0.01535 =
0.01419 0.00038 0.00066 0.00048
N2B 5 0.803684 0.367168 0.598576 11.00000 0.01535 0.01456 =
0.01597 0.00026 0.00203 0.00030
C1C 1 0.347505 0.641980 0.684088 11.00000 0.01558 0.01702 =
0.02329 -0.00123 0.00381 0.00072
AFIX 43
H1C 2 0.274456 0.682681 0.678475 11.00000 -1.20000
AFIX 0
C2C 1 0.395659 0.606877 0.727573 11.00000 0.02138 0.02050 =
0.01882 -0.00204 0.00665 -0.00094
AFIX 43
H2C 2 0.362950 0.619105 0.757667 11.00000 -1.20000
AFIX 0
C3C 1 0.502829 0.549377 0.718473 11.00000 0.02078 0.01663 =
0.01550 0.00049 0.00046 -0.00117
AFIX 43
H3C 2 0.554143 0.515443 0.742204 11.00000 -1.20000
AFIX 0
C5C 1 0.672174 0.552119 0.533582 11.00000 0.01631 0.01710 =
0.01778 -0.00047 0.00243 -0.00117
AFIX 43
H5C 2 0.750934 0.520040 0.529158 11.00000 -1.20000
AFIX 0
C6C 1 0.602080 0.606153 0.497610 11.00000 0.02284 0.02034 =
0.01413 0.00237 0.00237 -0.00213
AFIX 43
H6C 2 0.625379 0.617575 0.466061 11.00000 -1.20000
AFIX 0
C7C 1 0.494426 0.638485 0.517367 11.00000 0.02032 0.01566 =
0.01748 0.00205 -0.00211 0.00103
AFIX 43
H7C 2 0.427388 0.675857 0.501906 11.00000 -1.20000
AFIX 0
C8C 1 0.416999 0.627324 0.600192 11.00000 0.01507 0.01248 =
0.01974 -0.00058 -0.00070 -0.00123
C9C 1 0.427565 0.605884 0.649311 11.00000 0.01321 0.01270 =
0.01948 -0.00026 0.00149 -0.00091
C10C 1 0.501398 0.605471 0.565892 11.00000 0.01542 0.01324 =
0.01761 0.00033 -0.00067 -0.00074
C11C 1 0.297273 0.680480 0.582583 11.00000 0.01604 0.02213 =
0.01519 0.00170 0.00266 0.00478
C12C 1 0.287970 0.782033 0.581003 11.00000 0.02258 0.02297 =
0.02163 -0.00135 0.00082 0.00412
C13C 1 0.178158 0.829292 0.562851 11.00000 0.03223 0.02448 =
0.02573 0.00246 0.00372 0.01413
C14C 1 0.074469 0.773897 0.546365 11.00000 0.01760 0.04389 =
0.02045 0.00545 0.00190 0.01473
C15C 1 0.079830 0.672679 0.547821 11.00000 0.01472 0.04135 =
0.01991 0.00366 0.00128 0.00014
C16C 1 0.190557 0.627388 0.565820 11.00000 0.01909 0.02506 =
0.02015 0.00247 0.00351 0.00037
F1C 3 0.388138 0.837645 0.596716 11.00000 0.03186 0.01875 =
0.03585 -0.00221 -0.00723 0.00239
F2C 3 0.172744 0.927708 0.560276 11.00000 0.04806 0.02596 =
0.04808 0.00009 -0.00551 0.02013
F3C 3 -0.031986 0.819596 0.529009 11.00000 0.02394 0.05857 =
0.03596 0.00757 -0.00090 0.02253
F4C 3 -0.021419 0.618612 0.532533 11.00000 0.01630 0.05618 =
0.03402 0.00852 -0.00516 -0.00675
F5C 3 0.193245 0.528012 0.567051 11.00000 0.02338 0.02449 =
0.03636 0.00282 -0.00216 -0.00490
N1C 5 0.523269 0.548617 0.671962 11.00000 0.01574 0.01460 =
0.01566 -0.00007 0.00063 0.00051
N2C 5 0.614591 0.551630 0.574309 11.00000 0.01460 0.01447 =
0.01491 0.00067 0.00062 0.00060
HKLF 4
REM kjf082q_a.res in P2(1)/n
REM R1 = 0.0204 for 7008 Fo > 4sig(Fo) and 0.0220 for all 7365 data
REM 604 parameters refined using 0 restraints
END
WGHT 0.0131 4.2719
REM Instructions for potential hydrogen bonds
HTAB C2A F3A_$2
HTAB C3A F3B_$1
EQIV $3 x-1, y, z
HTAB C5A F2A_$3
EQIV $4 -x+3/2, y-1/2, -z+3/2
HTAB C6A N1A_$4
HTAB C1B F4A_$4
EQIV $5 -x+1, -y, -z+1
HTAB C1B F2B_$5
REM Highest difference peak 0.311, deepest hole -0.339, 1-sigma level 0.048
Q1 1 0.6837 0.1562 0.5890 11.00000 0.05 0.31
Q2 1 0.5073 0.2123 0.6042 11.00000 0.05 0.28
Q3 1 0.7417 0.0772 0.5970 11.00000 0.05 0.27
Q4 1 0.8463 0.2371 0.5851 11.00000 0.05 0.27
Q5 1 0.6961 0.0121 0.5351 11.00000 0.05 0.26
Q6 1 0.7543 -0.0747 0.5874 11.00000 0.05 0.26
Q7 1 0.3518 0.6517 0.5922 11.00000 0.05 0.25
Q8 1 0.3808 0.6164 0.6632 11.00000 0.05 0.25
Q9 1 0.7398 0.2385 0.5942 11.00000 0.05 0.25
Q10 1 0.5048 0.6323 0.5459 11.00000 0.05 0.25
Q11 1 0.9998 0.4372 0.7357 11.00000 0.05 0.24
Q12 1 0.8794 0.5399 0.6775 11.00000 0.05 0.24
Q13 1 0.6903 0.0855 0.5609 11.00000 0.05 0.24
Q14 1 0.0948 0.7214 0.5372 11.00000 0.05 0.24
Q15 1 0.6632 -0.0679 0.5520 11.00000 0.05 0.24
Q16 1 0.6438 0.5219 0.5977 11.00000 0.05 0.24
Q17 1 0.8640 0.3284 0.7384 11.00000 0.05 0.23
Q18 1 0.7864 0.3727 0.7168 11.00000 0.05 0.23
Q19 1 0.9842 0.5548 0.6916 11.00000 0.05 0.23
Q20 1 0.4747 0.5769 0.6598 11.00000 0.05 0.23
;
_shelx_res_checksum 6345
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN micromount using oil'
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_kjf115
_database_code_depnum_ccdc_archive 'CCDC 1841033'
_audit_update_record
;
2018-05-02 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;
_audit_creation_date 2018-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic
{Tris[5-(4-butyloxytetrafluorophenyl)dipyrrin]}-iron(III)
_chemical_formula_moiety 'C57 H45 F12 Fe1 N6 O3'
_chemical_formula_sum 'C57 H45 F12 Fe N6 O3'
_chemical_formula_weight 1145.84
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system trigonal
_space_group_IT_number 148
_space_group_name_H-M_alt 'R -3'
_space_group_name_Hall '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
_cell_length_a 24.0020(11)
_cell_length_b 24.0020(11)
_cell_length_c 15.1852(9)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 7576.1(8)
_cell_formula_units_Z 6
_cell_measurement_reflns_used 6014
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 69.05
_cell_measurement_theta_min 3.60
_shelx_estimated_absorpt_T_max 0.938
_shelx_estimated_absorpt_T_min 0.246
_exptl_absorpt_coefficient_mu 3.253
_exptl_absorpt_correction_T_max 0.7532
_exptl_absorpt_correction_T_min 0.2921
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1629 before and 0.1117 after correction. The Ratio of minimum to maximum transmission is 0.3878. The \l/2 correction factor is 0.00150.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.507
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Needle
_exptl_crystal_F_000 3522
_exptl_crystal_preparation ?
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and methanol by slow evaporation'
_exptl_crystal_size_max 0.6
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.02
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1428
_diffrn_reflns_av_unetI/netI 0.0980
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_k_min -28
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 31292
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 69.200
_diffrn_reflns_theta_min 3.605
_diffrn_ambient_temperature 100.01
_diffrn_detector 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker APEX2 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2541
_reflns_number_total 3129
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection 'APEX 3 (Bruker, 2016) '
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XT (Sheldrick, 2015)'
_refine_diff_density_max 0.467
_refine_diff_density_min -0.514
_refine_diff_density_rms 0.086
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.056
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 239
_refine_ls_number_reflns 3129
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0739
_refine_ls_R_factor_gt 0.0605
_refine_ls_restrained_S_all 1.056
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+14.2689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1562
_refine_ls_wR_factor_ref 0.1686
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.37854(15) 0.54019(15) 0.2807(2) 0.0226(6) Uani 1 1 d . . . . .
H1 H 0.3757 0.4999 0.2700 0.027 Uiso 1 1 calc R . . . .
C2 C 0.41516(15) 0.59607(15) 0.2351(2) 0.0234(6) Uani 1 1 d . . . . .
H2 H 0.4425 0.6018 0.1865 0.028 Uiso 1 1 calc R . . . .
C3 C 0.40469(15) 0.64347(16) 0.27376(19) 0.0231(6) Uani 1 1 d . . . . .
H3 H 0.4248 0.6870 0.2550 0.028 Uiso 1 1 calc R . . . .
C5 C 0.24196(15) 0.58584(15) 0.5536(2) 0.0232(7) Uani 1 1 d . . . . .
H5 H 0.2390 0.6211 0.5764 0.028 Uiso 1 1 calc R . . . .
C6 C 0.20674(16) 0.52249(16) 0.5855(2) 0.0255(7) Uani 1 1 d . . . . .
H6 H 0.1768 0.5079 0.6327 0.031 Uiso 1 1 calc R . . . .
C7 C 0.22374(15) 0.48572(15) 0.53539(19) 0.0233(7) Uani 1 1 d . . . . .
H7 H 0.2075 0.4408 0.5410 0.028 Uiso 1 1 calc R . . . .
C8 C 0.30186(14) 0.51209(14) 0.40989(19) 0.0189(6) Uani 1 1 d . . . . .
C9 C 0.34538(14) 0.55409(14) 0.34751(19) 0.0195(6) Uani 1 1 d . . . . .
C10 C 0.27042(15) 0.52785(14) 0.47327(19) 0.0199(6) Uani 1 1 d . . . . .
C11 C 0.28870(15) 0.44424(14) 0.4078(2) 0.0212(6) Uani 1 1 d . . . . .
C12 C 0.30879(16) 0.41969(16) 0.4752(2) 0.0255(7) Uani 1 1 d . . . . .
C13 C 0.29633(17) 0.35650(17) 0.4740(2) 0.0295(7) Uani 1 1 d . . . . .
C14 C 0.26336(17) 0.31497(16) 0.4048(2) 0.0289(7) Uani 1 1 d . . . . .
C15 C 0.24331(16) 0.33970(15) 0.3369(2) 0.0256(7) Uani 1 1 d . . . . .
C16 C 0.25615(15) 0.40276(14) 0.33877(19) 0.0219(6) Uani 1 1 d . . . . .
C17 C 0.2604(2) 0.22350(17) 0.3346(2) 0.0357(8) Uani 1 1 d . . . . .
H17A H 0.2772 0.2546 0.2853 0.043 Uiso 1 1 calc R . . . .
H17B H 0.2191 0.1860 0.3159 0.043 Uiso 1 1 calc R . . . .
C18 C 0.30748(17) 0.20216(18) 0.3572(2) 0.0328(8) Uani 1 1 d . . . . .
H18A H 0.2919 0.1734 0.4092 0.039 Uiso 1 1 calc R . . . .
H18B H 0.3494 0.2401 0.3726 0.039 Uiso 1 1 calc R . . . .
C19 C 0.31632(17) 0.16679(17) 0.2801(2) 0.0317(8) Uani 1 1 d . . . . .
H19A H 0.2736 0.1319 0.2608 0.038 Uiso 1 1 calc R . . . .
H19B H 0.3358 0.1971 0.2303 0.038 Uiso 1 1 calc R . . . .
C20 C 0.3583(2) 0.1380(2) 0.3018(3) 0.0506(11) Uani 1 1 d . . . . .
H20A H 0.3614 0.1152 0.2502 0.076 Uiso 1 1 calc GR . . . .
H20B H 0.3393 0.1078 0.3510 0.076 Uiso 1 1 calc GR . . . .
H20C H 0.4014 0.1725 0.3184 0.076 Uiso 1 1 calc GR . . . .
F1 F 0.34272(10) 0.45676(10) 0.54298(12) 0.0332(5) Uani 1 1 d . . . . .
F2 F 0.31744(12) 0.33547(11) 0.54127(14) 0.0426(6) Uani 1 1 d . . . . .
F3 F 0.20952(10) 0.30226(9) 0.26902(13) 0.0336(5) Uani 1 1 d . . . . .
F4 F 0.23274(9) 0.42205(9) 0.27264(12) 0.0266(4) Uani 1 1 d . . . . .
Fe1 Fe 0.3333 0.6667 0.41433(5) 0.0172(2) Uani 1 3 d S T P . .
N1 N 0.36259(12) 0.61881(12) 0.34060(16) 0.0201(5) Uani 1 1 d . . . . .
N2 N 0.28048(12) 0.58986(12) 0.48677(16) 0.0207(5) Uani 1 1 d . . . . .
O1 O 0.25003(15) 0.25353(12) 0.41165(17) 0.0455(8) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0226(15) 0.0229(15) 0.0243(15) -0.0004(12) -0.0015(12) 0.0129(13)
C2 0.0242(16) 0.0286(17) 0.0203(14) 0.0001(12) 0.0017(12) 0.0155(14)
C3 0.0220(16) 0.0269(16) 0.0211(14) 0.0011(12) 0.0023(12) 0.0127(13)
C5 0.0243(16) 0.0246(16) 0.0216(14) -0.0001(12) 0.0029(12) 0.0128(13)
C6 0.0244(16) 0.0294(17) 0.0226(15) 0.0044(12) 0.0059(12) 0.0135(14)
C7 0.0239(16) 0.0195(15) 0.0249(15) 0.0044(12) 0.0018(12) 0.0096(13)
C8 0.0188(14) 0.0171(14) 0.0212(14) -0.0004(11) -0.0031(11) 0.0093(12)
C9 0.0185(14) 0.0191(15) 0.0201(14) 0.0015(11) -0.0006(11) 0.0087(12)
C10 0.0215(15) 0.0175(14) 0.0193(14) 0.0002(11) -0.0005(11) 0.0086(12)
C11 0.0237(15) 0.0184(15) 0.0245(14) 0.0020(11) 0.0035(12) 0.0128(13)
C12 0.0283(17) 0.0272(17) 0.0252(15) 0.0011(12) 0.0000(13) 0.0169(14)
C13 0.0388(19) 0.0313(18) 0.0261(16) 0.0097(13) 0.0068(14) 0.0234(16)
C14 0.0367(19) 0.0204(16) 0.0333(17) 0.0084(13) 0.0154(14) 0.0172(15)
C15 0.0263(16) 0.0227(16) 0.0254(15) -0.0020(12) 0.0049(13) 0.0104(14)
C16 0.0254(16) 0.0185(15) 0.0214(14) 0.0037(11) 0.0030(12) 0.0107(13)
C17 0.056(2) 0.0257(18) 0.0343(18) 0.0066(14) 0.0158(17) 0.0266(18)
C18 0.0299(18) 0.0297(18) 0.0350(18) -0.0033(14) 0.0049(14) 0.0120(15)
C19 0.0319(18) 0.0286(18) 0.0354(18) -0.0032(14) 0.0029(14) 0.0157(15)
C20 0.052(3) 0.075(3) 0.044(2) -0.018(2) -0.0114(19) 0.047(3)
F1 0.0371(11) 0.0401(12) 0.0279(10) -0.0031(8) -0.0088(8) 0.0235(10)
F2 0.0610(15) 0.0487(13) 0.0378(11) 0.0143(10) 0.0035(10) 0.0422(12)
F3 0.0371(11) 0.0217(10) 0.0335(10) -0.0053(8) 0.0043(8) 0.0082(8)
F4 0.0296(10) 0.0255(10) 0.0237(9) 0.0022(7) -0.0032(7) 0.0130(8)
Fe1 0.0176(3) 0.0176(3) 0.0163(4) 0.000 0.000 0.00882(15)
N1 0.0172(12) 0.0212(13) 0.0199(12) 0.0024(10) -0.0004(9) 0.0081(11)
N2 0.0218(13) 0.0229(13) 0.0186(12) -0.0029(10) -0.0003(10) 0.0121(11)
O1 0.079(2) 0.0297(14) 0.0412(14) 0.0143(11) 0.0310(14) 0.0370(15)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9500 . ?
C1 C2 1.369(4) . ?
C1 C9 1.428(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.410(4) . ?
C3 H3 0.9500 . ?
C3 N1 1.343(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.405(5) . ?
C5 N2 1.344(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.372(4) . ?
C7 H7 0.9500 . ?
C7 C10 1.427(4) . ?
C8 C9 1.397(4) . ?
C8 C10 1.387(4) . ?
C8 C11 1.496(4) . ?
C9 N1 1.398(4) . ?
C10 N2 1.399(4) . ?
C11 C12 1.382(4) . ?
C11 C16 1.386(4) . ?
C12 C13 1.392(5) . ?
C12 F1 1.338(4) . ?
C13 C14 1.391(5) . ?
C13 F2 1.346(4) . ?
C14 C15 1.390(5) . ?
C14 O1 1.348(4) . ?
C15 C16 1.386(4) . ?
C15 F3 1.341(4) . ?
C16 F4 1.341(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.496(5) . ?
C17 O1 1.458(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.523(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.516(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Fe1 N1 1.968(3) 3_565 ?
Fe1 N1 1.968(3) 2_665 ?
Fe1 N1 1.968(3) . ?
Fe1 N2 1.970(3) 3_565 ?
Fe1 N2 1.970(3) . ?
Fe1 N2 1.970(3) 2_665 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 126.6 . . ?
C2 C1 C9 106.9(3) . . ?
C9 C1 H1 126.6 . . ?
C1 C2 H2 126.5 . . ?
C1 C2 C3 107.1(3) . . ?
C3 C2 H2 126.5 . . ?
C2 C3 H3 124.5 . . ?
N1 C3 C2 111.0(3) . . ?
N1 C3 H3 124.5 . . ?
C6 C5 H5 124.5 . . ?
N2 C5 H5 124.5 . . ?
N2 C5 C6 110.9(3) . . ?
C5 C6 H6 126.5 . . ?
C7 C6 C5 107.1(3) . . ?
C7 C6 H6 126.5 . . ?
C6 C7 H7 126.5 . . ?
C6 C7 C10 106.9(3) . . ?
C10 C7 H7 126.5 . . ?
C9 C8 C11 116.5(3) . . ?
C10 C8 C9 125.9(3) . . ?
C10 C8 C11 117.6(3) . . ?
C8 C9 C1 128.0(3) . . ?
C8 C9 N1 123.5(3) . . ?
N1 C9 C1 108.5(3) . . ?
C8 C10 C7 127.4(3) . . ?
C8 C10 N2 124.3(3) . . ?
N2 C10 C7 108.3(3) . . ?
C12 C11 C8 121.3(3) . . ?
C12 C11 C16 116.4(3) . . ?
C16 C11 C8 122.3(3) . . ?
C11 C12 C13 121.6(3) . . ?
F1 C12 C11 120.8(3) . . ?
F1 C12 C13 117.5(3) . . ?
C14 C13 C12 121.7(3) . . ?
F2 C13 C12 118.9(3) . . ?
F2 C13 C14 119.4(3) . . ?
C15 C14 C13 116.7(3) . . ?
O1 C14 C13 117.7(3) . . ?
O1 C14 C15 125.5(3) . . ?
C16 C15 C14 121.0(3) . . ?
F3 C15 C14 120.4(3) . . ?
F3 C15 C16 118.5(3) . . ?
C15 C16 C11 122.5(3) . . ?
F4 C16 C11 120.1(3) . . ?
F4 C16 C15 117.3(3) . . ?
H17A C17 H17B 108.3 . . ?
C18 C17 H17A 109.8 . . ?
C18 C17 H17B 109.8 . . ?
O1 C17 H17A 109.8 . . ?
O1 C17 H17B 109.8 . . ?
O1 C17 C18 109.3(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 C19 110.8(3) . . ?
H18A C18 H18B 108.1 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C18 C19 H19A 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 C18 113.3(3) . . ?
C20 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 Fe1 N1 90.82(10) 3_565 2_665 ?
N1 Fe1 N1 90.83(10) 2_665 . ?
N1 Fe1 N1 90.83(10) 3_565 . ?
N1 Fe1 N2 86.17(10) 2_665 3_565 ?
N1 Fe1 N2 86.17(10) . 2_665 ?
N1 Fe1 N2 176.36(10) . 3_565 ?
N1 Fe1 N2 91.27(10) . . ?
N1 Fe1 N2 91.27(10) 3_565 3_565 ?
N1 Fe1 N2 91.27(10) 2_665 2_665 ?
N1 Fe1 N2 176.36(10) 2_665 . ?
N1 Fe1 N2 176.36(10) 3_565 2_665 ?
N1 Fe1 N2 86.17(10) 3_565 . ?
N2 Fe1 N2 91.84(10) 3_565 2_665 ?
N2 Fe1 N2 91.84(10) . 2_665 ?
N2 Fe1 N2 91.84(10) 3_565 . ?
C3 N1 C9 106.6(3) . . ?
C3 N1 Fe1 125.6(2) . . ?
C9 N1 Fe1 127.8(2) . . ?
C5 N2 C10 106.7(3) . . ?
C5 N2 Fe1 126.0(2) . . ?
C10 N2 Fe1 127.0(2) . . ?
C14 O1 C17 118.2(3) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2 F4 0.95 2.41 3.292(3) 154.3 15
C17 H17A F2 0.99 2.38 3.315(4) 157.2 9_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
C1 C2 C3 N1 -0.7(4) . . . . ?
C1 C9 N1 C3 -0.7(3) . . . . ?
C1 C9 N1 Fe1 -179.6(2) . . . . ?
C2 C1 C9 C8 179.3(3) . . . . ?
C2 C1 C9 N1 0.3(3) . . . . ?
C2 C3 N1 C9 0.9(3) . . . . ?
C2 C3 N1 Fe1 179.8(2) . . . . ?
C5 C6 C7 C10 0.7(4) . . . . ?
C6 C5 N2 C10 0.4(4) . . . . ?
C6 C5 N2 Fe1 174.4(2) . . . . ?
C6 C7 C10 C8 179.1(3) . . . . ?
C6 C7 C10 N2 -0.4(3) . . . . ?
C7 C10 N2 C5 0.0(3) . . . . ?
C7 C10 N2 Fe1 -173.9(2) . . . . ?
C8 C9 N1 C3 -179.7(3) . . . . ?
C8 C9 N1 Fe1 1.3(4) . . . . ?
C8 C10 N2 C5 -179.6(3) . . . . ?
C8 C10 N2 Fe1 6.5(4) . . . . ?
C8 C11 C12 C13 179.5(3) . . . . ?
C8 C11 C12 F1 -2.4(5) . . . . ?
C8 C11 C16 C15 -179.4(3) . . . . ?
C8 C11 C16 F4 -2.9(5) . . . . ?
C9 C1 C2 C3 0.3(3) . . . . ?
C9 C8 C10 C7 177.1(3) . . . . ?
C9 C8 C10 N2 -3.4(5) . . . . ?
C9 C8 C11 C12 111.8(3) . . . . ?
C9 C8 C11 C16 -68.0(4) . . . . ?
C10 C8 C9 C1 -179.5(3) . . . . ?
C10 C8 C9 N1 -0.7(5) . . . . ?
C10 C8 C11 C12 -67.9(4) . . . . ?
C10 C8 C11 C16 112.3(3) . . . . ?
C11 C8 C9 C1 0.9(4) . . . . ?
C11 C8 C9 N1 179.7(3) . . . . ?
C11 C8 C10 C7 -3.3(5) . . . . ?
C11 C8 C10 N2 176.2(3) . . . . ?
C11 C12 C13 C14 0.3(5) . . . . ?
C11 C12 C13 F2 179.6(3) . . . . ?
C12 C11 C16 C15 0.8(5) . . . . ?
C12 C11 C16 F4 177.2(3) . . . . ?
C12 C13 C14 C15 -0.2(5) . . . . ?
C12 C13 C14 O1 -176.1(3) . . . . ?
C13 C14 C15 C16 0.3(5) . . . . ?
C13 C14 C15 F3 -178.0(3) . . . . ?
C13 C14 O1 C17 -136.3(4) . . . . ?
C14 C15 C16 C11 -0.6(5) . . . . ?
C14 C15 C16 F4 -177.2(3) . . . . ?
C15 C14 O1 C17 48.2(5) . . . . ?
C16 C11 C12 C13 -0.6(5) . . . . ?
C16 C11 C12 F1 177.4(3) . . . . ?
C17 C18 C19 C20 -174.2(3) . . . . ?
C18 C17 O1 C14 121.1(4) . . . . ?
F1 C12 C13 C14 -177.8(3) . . . . ?
F1 C12 C13 F2 1.5(5) . . . . ?
F2 C13 C14 C15 -179.4(3) . . . . ?
F2 C13 C14 O1 4.7(5) . . . . ?
F3 C15 C16 C11 177.6(3) . . . . ?
F3 C15 C16 F4 1.1(4) . . . . ?
N2 C5 C6 C7 -0.7(4) . . . . ?
O1 C14 C15 C16 175.8(3) . . . . ?
O1 C14 C15 F3 -2.4(5) . . . . ?
O1 C17 C18 C19 176.5(3) . . . . ?
_shelx_res_file
;
kjf115.res created by SHELXL-2014/7
TITL kjf115_a.res in R-3
REM Old TITL kjf115 in R-3 #148
REM SHELXT solution in R-3
REM R1 0.128, Rweak 0.012, Alpha 0.034, Orientation as input
REM Formula found by SHELXT: C57 N9 F12 Fe
CELL 1.54178 24.002 24.002 15.1852 90 90 120
ZERR 6 0.0011 0.0011 0.0009 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H F Fe N O
UNIT 342 270 72 6 36 18
EQIV $1 0.667-Y+X,0.333+X,0.333-Z
EQIV $2 0.333+Y-X,0.667-X,-0.333+Z
L.S. 10
PLAN 20
SIZE 0.02 0.06 0.6
TEMP -173.14
HTAB C2 F4_$1
HTAB C17 F2_$2
BOND $H
WPDB
HTAB
MORE -1
CONF
fmap 2
acta
OMIT 0 25 2
REM
REM
REM
WGHT 0.074300 14.268901
FVAR 0.16154
C1 1 0.378543 0.540186 0.280711 11.00000 0.02255 0.02293 =
0.02434 -0.00044 -0.00147 0.01288
AFIX 43
H1 2 0.375727 0.499858 0.270004 11.00000 -1.20000
AFIX 0
C2 1 0.415158 0.596069 0.235076 11.00000 0.02423 0.02865 =
0.02026 0.00007 0.00170 0.01550
AFIX 43
H2 2 0.442475 0.601838 0.186494 11.00000 -1.20000
AFIX 0
C3 1 0.404694 0.643469 0.273759 11.00000 0.02200 0.02688 =
0.02105 0.00111 0.00229 0.01271
AFIX 43
H3 2 0.424753 0.687033 0.255042 11.00000 -1.20000
AFIX 0
C5 1 0.241965 0.585836 0.553649 11.00000 0.02434 0.02461 =
0.02156 -0.00012 0.00290 0.01282
AFIX 43
H5 2 0.238953 0.621112 0.576381 11.00000 -1.20000
AFIX 0
C6 1 0.206741 0.522489 0.585457 11.00000 0.02444 0.02942 =
0.02261 0.00439 0.00594 0.01345
AFIX 43
H6 2 0.176799 0.507869 0.632719 11.00000 -1.20000
AFIX 0
C7 1 0.223735 0.485717 0.535394 11.00000 0.02386 0.01951 =
0.02494 0.00437 0.00179 0.00964
AFIX 43
H7 2 0.207503 0.440773 0.541033 11.00000 -1.20000
AFIX 0
C8 1 0.301857 0.512088 0.409888 11.00000 0.01879 0.01708 =
0.02118 -0.00038 -0.00307 0.00930
C9 1 0.345376 0.554087 0.347508 11.00000 0.01853 0.01905 =
0.02007 0.00148 -0.00063 0.00869
C10 1 0.270422 0.527847 0.473274 11.00000 0.02149 0.01746 =
0.01928 0.00020 -0.00053 0.00859
C11 1 0.288702 0.444243 0.407793 11.00000 0.02368 0.01844 =
0.02448 0.00197 0.00347 0.01279
C12 1 0.308790 0.419695 0.475172 11.00000 0.02828 0.02720 =
0.02516 0.00113 -0.00001 0.01689
C13 1 0.296335 0.356503 0.473988 11.00000 0.03879 0.03130 =
0.02612 0.00966 0.00678 0.02339
C14 1 0.263357 0.314966 0.404766 11.00000 0.03669 0.02044 =
0.03333 0.00843 0.01543 0.01721
C15 1 0.243312 0.339701 0.336878 11.00000 0.02631 0.02274 =
0.02543 -0.00204 0.00490 0.01042
C16 1 0.256148 0.402762 0.338774 11.00000 0.02542 0.01852 =
0.02137 0.00365 0.00297 0.01068
C17 1 0.260361 0.223496 0.334647 11.00000 0.05558 0.02574 =
0.03434 0.00661 0.01585 0.02665
AFIX 23
H17A 2 0.277169 0.254623 0.285341 11.00000 -1.20000
H17B 2 0.219091 0.186025 0.315918 11.00000 -1.20000
AFIX 0
C18 1 0.307483 0.202159 0.357237 11.00000 0.02991 0.02971 =
0.03498 -0.00326 0.00491 0.01200
AFIX 23
H18A 2 0.291852 0.173387 0.409154 11.00000 -1.20000
H18B 2 0.349403 0.240106 0.372625 11.00000 -1.20000
AFIX 0
C19 1 0.316321 0.166789 0.280072 11.00000 0.03190 0.02861 =
0.03542 -0.00322 0.00288 0.01573
AFIX 23
H19A 2 0.273566 0.131934 0.260800 11.00000 -1.20000
H19B 2 0.335809 0.197121 0.230274 11.00000 -1.20000
AFIX 0
C20 1 0.358329 0.138035 0.301839 11.00000 0.05226 0.07485 =
0.04439 -0.01823 -0.01140 0.04656
AFIX 137
H20A 2 0.361444 0.115248 0.250204 11.00000 -1.50000
H20B 2 0.339305 0.107806 0.350978 11.00000 -1.50000
H20C 2 0.401394 0.172461 0.318408 11.00000 -1.50000
AFIX 0
F1 3 0.342720 0.456762 0.542982 11.00000 0.03715 0.04015 =
0.02791 -0.00311 -0.00876 0.02348
F2 3 0.317443 0.335474 0.541270 11.00000 0.06104 0.04866 =
0.03782 0.01425 0.00351 0.04221
F3 3 0.209523 0.302264 0.269019 11.00000 0.03713 0.02170 =
0.03349 -0.00530 0.00427 0.00825
F4 3 0.232742 0.422049 0.272644 11.00000 0.02961 0.02553 =
0.02372 0.00221 -0.00320 0.01304
FE1 4 0.333333 0.666667 0.414332 10.33333 0.01764 0.01764 =
0.01628 0.00000 0.00000 0.00882
N1 5 0.362586 0.618810 0.340595 11.00000 0.01718 0.02117 =
0.01993 0.00241 -0.00036 0.00813
N2 5 0.280485 0.589856 0.486774 11.00000 0.02178 0.02289 =
0.01859 -0.00294 -0.00027 0.01207
O1 6 0.250028 0.253531 0.411650 11.00000 0.07879 0.02970 =
0.04123 0.01431 0.03098 0.03700
HKLF 4
REM kjf115_a.res in R-3
REM R1 = 0.0605 for 2541 Fo > 4sig(Fo) and 0.0739 for all 3129 data
REM 239 parameters refined using 0 restraints
END
WGHT 0.0743 14.2854
REM Instructions for potential hydrogen bonds
HTAB C2 F4_$1
HTAB C17 F2_$2
REM Highest difference peak 0.467, deepest hole -0.514, 1-sigma level 0.086
Q1 1 0.3062 0.6162 0.4495 11.00000 0.05 0.47
Q2 1 0.3612 0.6392 0.3913 11.00000 0.05 0.46
Q3 1 0.2863 0.6213 0.4545 11.00000 0.05 0.44
Q4 1 0.3246 0.6201 0.3687 11.00000 0.05 0.37
Q5 1 0.2327 0.3258 0.2141 11.00000 0.05 0.33
Q6 1 0.3191 0.5670 0.3726 11.00000 0.05 0.30
Q7 1 0.3591 0.5843 0.3667 11.00000 0.05 0.30
Q8 1 0.2461 0.4417 0.2139 11.00000 0.05 0.29
Q9 1 0.3845 0.1460 0.3576 11.00000 0.05 0.28
Q10 1 0.2523 0.5501 0.6052 11.00000 0.05 0.28
Q11 1 0.2745 0.5605 0.4645 11.00000 0.05 0.27
Q12 1 0.3983 0.5131 0.1662 11.00000 0.05 0.27
Q13 1 0.3103 0.1894 0.2243 11.00000 0.05 0.27
Q14 1 0.3333 0.6667 0.3527 10.33333 0.05 0.26
Q15 1 0.2497 0.6086 0.5161 11.00000 0.05 0.26
Q16 1 0.3029 0.3458 0.5003 11.00000 0.05 0.26
Q17 1 0.4603 0.7106 0.2736 11.00000 0.05 0.26
Q18 1 0.3780 0.6363 0.3041 11.00000 0.05 0.25
Q19 1 0.3154 0.6047 0.5358 11.00000 0.05 0.25
Q20 1 0.3001 0.3480 0.4273 11.00000 0.05 0.25
;
_shelx_res_checksum 16383
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN micromount using oil'
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT978_kjf115
;
PROBLEM: Number C-C Bonds with Positive Residual Density. 0 Info
RESPONSE: Due to weak high angle data.
;
_vrf_RINTA01_kjf115
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: Rint is greater than 0.12 due to weak data.
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_kjf138_a
_database_code_depnum_ccdc_archive 'CCDC 1841036'
_audit_update_record
;
2018-05-02 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;
_audit_creation_date 2018-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic
Tris[5-(pentafluorophenyl)dipyrrin]gallium(III)
_chemical_formula_moiety 'C45 H18 F15 Ga N6'
_chemical_formula_sum 'C45 H18 F15 Ga N6'
_chemical_formula_weight 997.37
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga -1.2846 0.7763 '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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_H-M_alt 'P b c a'
_space_group_name_Hall '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
_cell_length_a 25.7650(8)
_cell_length_b 8.8371(3)
_cell_length_c 35.7783(11)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 8146.3(5)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 8529
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 67.02
_cell_measurement_theta_min 2.47
_shelx_estimated_absorpt_T_max 0.845
_shelx_estimated_absorpt_T_min 0.534
_exptl_absorpt_coefficient_mu 1.940
_exptl_absorpt_correction_T_max 0.7531
_exptl_absorpt_correction_T_min 0.6044
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1280 before and 0.0715 after correction. The Ratio of minimum to maximum transmission is 0.8025. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light orange'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.626
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Plate
_exptl_crystal_F_000 3968
_exptl_crystal_preparation ?
_exptl_crystal_recrystallization_method
'The material was recrystallised from DCM by slow evaporation'
_exptl_crystal_size_max 0.37
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.09
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0834
_diffrn_reflns_av_unetI/netI 0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_h_min -30
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 42
_diffrn_reflns_limit_l_min -43
_diffrn_reflns_number 52826
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 68.293
_diffrn_reflns_theta_min 2.470
_diffrn_ambient_temperature 100(2)
_diffrn_detector 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker SMART APEX2 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_diffrn_special_details ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5728
_reflns_number_total 7436
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection 'APEX 3 (Bruker, 2016)'
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XT (Sheldrick, 2015)'
_refine_diff_density_max 0.587
_refine_diff_density_min -0.443
_refine_diff_density_rms 0.080
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.044
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 604
_refine_ls_number_reflns 7436
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0679
_refine_ls_R_factor_gt 0.0477
_refine_ls_restrained_S_all 1.044
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+11.7158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1127
_refine_ls_wR_factor_ref 0.1234
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C1A(H1A), C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C7A(H7A), C1B(H1B),
C2B(H2B), C3B(H3B), C5B(H5B), C6B(H6B), C7B(H7B), C1C(H1C), C2C(H2C), C3C(H3C),
C5C(H5C), C6C(H6C), C7C(H7C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.59999(2) 0.45853(4) 0.40909(2) 0.01575(11) Uani 1 1 d . . . . .
C1A C 0.64743(12) 0.3541(4) 0.29711(9) 0.0206(7) Uani 1 1 d . . . . .
H1A H 0.6581 0.3814 0.2726 0.025 Uiso 1 1 calc R . . . .
C2A C 0.63179(13) 0.2140(4) 0.30874(10) 0.0230(7) Uani 1 1 d . . . . .
H2A H 0.6295 0.1252 0.2939 0.028 Uiso 1 1 calc R . . . .
C3A C 0.61964(13) 0.2264(4) 0.34707(9) 0.0207(7) Uani 1 1 d . . . . .
H3A H 0.6078 0.1451 0.3622 0.025 Uiso 1 1 calc R . . . .
C5A C 0.64536(12) 0.7723(4) 0.41963(9) 0.0201(7) Uani 1 1 d . . . . .
H5A H 0.6349 0.7737 0.4451 0.024 Uiso 1 1 calc R . . . .
C6A C 0.66914(13) 0.8944(4) 0.40131(10) 0.0230(7) Uani 1 1 d . . . . .
H6A H 0.6778 0.9897 0.4119 0.028 Uiso 1 1 calc R . . . .
C7A C 0.67749(12) 0.8483(4) 0.36488(10) 0.0209(7) Uani 1 1 d . . . . .
H7A H 0.6927 0.9065 0.3454 0.025 Uiso 1 1 calc R . . . .
C8A C 0.65937(12) 0.6034(4) 0.33073(9) 0.0179(6) Uani 1 1 d . . . . .
C9A C 0.64469(12) 0.4518(4) 0.32888(9) 0.0182(6) Uani 1 1 d . . . . .
C10A C 0.65881(12) 0.6969(4) 0.36213(9) 0.0188(7) Uani 1 1 d . . . . .
C11A C 0.67793(12) 0.6737(3) 0.29506(9) 0.0180(7) Uani 1 1 d . . . . .
C12A C 0.72628(12) 0.6413(3) 0.27981(9) 0.0187(7) Uani 1 1 d . . . . .
C13A C 0.74339(12) 0.7034(4) 0.24676(9) 0.0198(7) Uani 1 1 d . . . . .
C14A C 0.71123(13) 0.8032(4) 0.22771(9) 0.0204(7) Uani 1 1 d . . . . .
C15A C 0.66306(13) 0.8378(3) 0.24185(9) 0.0206(7) Uani 1 1 d . . . . .
C16A C 0.64718(12) 0.7740(4) 0.27520(9) 0.0200(7) Uani 1 1 d . . . . .
F1A F 0.75771(7) 0.5435(2) 0.29747(5) 0.0235(4) Uani 1 1 d . . . . .
F2A F 0.78978(7) 0.6678(2) 0.23289(5) 0.0253(4) Uani 1 1 d . . . . .
F3A F 0.72680(8) 0.8620(2) 0.19513(5) 0.0288(5) Uani 1 1 d . . . . .
F4A F 0.63176(8) 0.9319(2) 0.22299(6) 0.0292(5) Uani 1 1 d . . . . .
F5A F 0.59965(7) 0.8104(2) 0.28793(6) 0.0280(4) Uani 1 1 d . . . . .
N1A N 0.62702(10) 0.3676(3) 0.35929(7) 0.0174(5) Uani 1 1 d . . . . .
N2A N 0.63918(10) 0.6538(3) 0.39688(7) 0.0173(5) Uani 1 1 d . . . . .
C1B C 0.55981(13) 0.6149(4) 0.51926(9) 0.0226(7) Uani 1 1 d . . . . .
H1B H 0.5643 0.6224 0.5455 0.027 Uiso 1 1 calc R . . . .
C2B C 0.52178(13) 0.6831(4) 0.49838(10) 0.0215(7) Uani 1 1 d . . . . .
H2B H 0.4951 0.7479 0.5074 0.026 Uiso 1 1 calc R . . . .
C3B C 0.52993(12) 0.6383(3) 0.46102(9) 0.0185(7) Uani 1 1 d . . . . .
H3B H 0.5086 0.6680 0.4407 0.022 Uiso 1 1 calc R . . . .
C5B C 0.70096(12) 0.2917(4) 0.42466(10) 0.0211(7) Uani 1 1 d . . . . .
H5B H 0.7071 0.2779 0.3987 0.025 Uiso 1 1 calc R . . . .
C6B C 0.73169(13) 0.2277(4) 0.45298(10) 0.0262(8) Uani 1 1 d . . . . .
H6B H 0.7610 0.1637 0.4498 0.031 Uiso 1 1 calc R . . . .
C7B C 0.71091(13) 0.2763(4) 0.48615(10) 0.0242(7) Uani 1 1 d . . . . .
H7B H 0.7232 0.2525 0.5105 0.029 Uiso 1 1 calc R . . . .
C8B C 0.63437(12) 0.4430(3) 0.50236(9) 0.0191(7) Uani 1 1 d . . . . .
C9B C 0.59127(12) 0.5307(3) 0.49399(9) 0.0189(7) Uani 1 1 d . . . . .
C10B C 0.66734(12) 0.3692(4) 0.47733(9) 0.0197(7) Uani 1 1 d . . . . .
C11B C 0.64699(13) 0.4229(4) 0.54301(9) 0.0212(7) Uani 1 1 d . . . . .
C12B C 0.62424(14) 0.3082(4) 0.56402(10) 0.0245(7) Uani 1 1 d . . . . .
C13B C 0.63705(15) 0.2851(4) 0.60120(10) 0.0300(8) Uani 1 1 d . . . . .
C14B C 0.67296(16) 0.3768(4) 0.61820(10) 0.0333(9) Uani 1 1 d . . . . .
C15B C 0.69597(15) 0.4911(4) 0.59817(10) 0.0326(9) Uani 1 1 d . . . . .
C16B C 0.68267(14) 0.5126(4) 0.56113(10) 0.0257(8) Uani 1 1 d . . . . .
F1B F 0.58945(8) 0.2159(2) 0.54802(6) 0.0347(5) Uani 1 1 d . . . . .
F2B F 0.61435(10) 0.1723(3) 0.62028(6) 0.0455(6) Uani 1 1 d . . . . .
F3B F 0.68496(11) 0.3546(3) 0.65402(6) 0.0498(7) Uani 1 1 d . . . . .
F4B F 0.73011(10) 0.5836(3) 0.61479(7) 0.0484(6) Uani 1 1 d . . . . .
F5B F 0.70552(9) 0.6272(2) 0.54277(6) 0.0374(5) Uani 1 1 d . . . . .
N1B N 0.57140(10) 0.5489(3) 0.45791(7) 0.0161(5) Uani 1 1 d . . . . .
N2B N 0.66199(10) 0.3747(3) 0.43862(7) 0.0179(6) Uani 1 1 d . . . . .
C1C C 0.50374(13) 0.0622(4) 0.41057(9) 0.0230(7) Uani 1 1 d . . . . .
H1C H 0.4762 0.0004 0.4017 0.028 Uiso 1 1 calc R . . . .
C2C C 0.53956(13) 0.0246(4) 0.43740(10) 0.0243(7) Uani 1 1 d . . . . .
H2C H 0.5413 -0.0678 0.4509 0.029 Uiso 1 1 calc R . . . .
C3C C 0.57315(12) 0.1488(4) 0.44108(9) 0.0198(7) Uani 1 1 d . . . . .
H3C H 0.6021 0.1521 0.4575 0.024 Uiso 1 1 calc R . . . .
C5C C 0.53163(13) 0.6763(4) 0.36334(9) 0.0233(7) Uani 1 1 d . . . . .
H5C H 0.5532 0.7603 0.3692 0.028 Uiso 1 1 calc R . . . .
C6C C 0.49029(14) 0.6812(4) 0.33771(10) 0.0290(8) Uani 1 1 d . . . . .
H6C H 0.4792 0.7664 0.3236 0.035 Uiso 1 1 calc R . . . .
C7C C 0.46904(14) 0.5380(4) 0.33698(10) 0.0300(8) Uani 1 1 d . . . . .
H7C H 0.4404 0.5056 0.3223 0.036 Uiso 1 1 calc R . . . .
C8C C 0.48971(13) 0.2985(4) 0.37197(9) 0.0208(7) Uani 1 1 d . . . . .
C9C C 0.51584(13) 0.2115(4) 0.39864(9) 0.0194(7) Uani 1 1 d . . . . .
C10C C 0.49816(13) 0.4482(4) 0.36244(9) 0.0209(7) Uani 1 1 d . . . . .
C11C C 0.44758(13) 0.2168(4) 0.35091(10) 0.0235(7) Uani 1 1 d . . . . .
C12C C 0.45788(14) 0.1460(4) 0.31725(11) 0.0323(9) Uani 1 1 d . . . . .
C13C C 0.42034(15) 0.0640(4) 0.29827(11) 0.0332(9) Uani 1 1 d . . . . .
C14C C 0.37160(14) 0.0520(4) 0.31284(10) 0.0275(8) Uani 1 1 d . . . . .
C15C C 0.35958(13) 0.1217(4) 0.34592(10) 0.0274(8) Uani 1 1 d . . . . .
C16C C 0.39790(13) 0.2018(4) 0.36474(10) 0.0255(7) Uani 1 1 d . . . . .
F1C F 0.50543(9) 0.1559(3) 0.30234(7) 0.0558(8) Uani 1 1 d . . . . .
F2C F 0.43199(10) -0.0021(3) 0.26554(7) 0.0575(8) Uani 1 1 d . . . . .
F3C F 0.33548(8) -0.0292(2) 0.29493(6) 0.0345(5) Uani 1 1 d . . . . .
F4C F 0.31250(8) 0.1069(3) 0.36054(7) 0.0454(6) Uani 1 1 d . . . . .
F5C F 0.38573(8) 0.2650(3) 0.39768(7) 0.0438(6) Uani 1 1 d . . . . .
N1C N 0.55911(10) 0.2620(3) 0.41836(7) 0.0178(6) Uani 1 1 d . . . . .
N2C N 0.53684(10) 0.5384(3) 0.37851(7) 0.0179(6) 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
Ga1 0.0167(2) 0.01241(19) 0.01817(19) 0.00116(15) 0.00031(15) -0.00086(15)
C1A 0.0219(17) 0.0186(16) 0.0213(16) -0.0003(13) 0.0007(13) 0.0021(13)
C2A 0.0241(18) 0.0177(16) 0.0274(18) -0.0043(13) 0.0021(14) -0.0008(13)
C3A 0.0222(17) 0.0130(16) 0.0269(17) 0.0039(13) 0.0007(13) 0.0004(13)
C5A 0.0205(17) 0.0182(16) 0.0216(16) -0.0016(13) 0.0000(12) 0.0013(13)
C6A 0.0230(18) 0.0155(16) 0.0306(18) -0.0012(13) -0.0015(14) -0.0024(13)
C7A 0.0179(17) 0.0157(16) 0.0290(18) 0.0072(13) 0.0031(13) -0.0005(13)
C8A 0.0148(16) 0.0161(16) 0.0229(16) 0.0040(13) -0.0007(12) 0.0018(12)
C9A 0.0178(16) 0.0160(16) 0.0209(16) 0.0010(13) 0.0010(12) 0.0031(13)
C10A 0.0168(16) 0.0181(16) 0.0215(16) 0.0025(13) 0.0008(13) 0.0008(13)
C11A 0.0194(17) 0.0135(15) 0.0210(16) 0.0002(12) -0.0004(12) -0.0020(12)
C12A 0.0227(17) 0.0154(15) 0.0181(15) 0.0002(12) -0.0019(13) -0.0004(13)
C13A 0.0187(17) 0.0184(16) 0.0224(16) -0.0021(13) 0.0018(13) -0.0016(13)
C14A 0.0261(18) 0.0183(16) 0.0166(15) 0.0020(12) 0.0007(13) -0.0065(13)
C15A 0.0235(18) 0.0151(16) 0.0231(17) 0.0062(13) -0.0064(13) 0.0008(13)
C16A 0.0175(17) 0.0148(15) 0.0278(17) 0.0014(13) 0.0009(13) 0.0012(12)
F1A 0.0215(10) 0.0233(10) 0.0257(10) 0.0063(8) 0.0000(8) 0.0058(8)
F2A 0.0250(11) 0.0255(10) 0.0253(10) -0.0004(8) 0.0069(8) -0.0003(8)
F3A 0.0363(12) 0.0295(11) 0.0204(10) 0.0080(8) 0.0025(8) -0.0032(9)
F4A 0.0286(11) 0.0264(11) 0.0326(11) 0.0120(8) -0.0075(9) 0.0026(8)
F5A 0.0211(10) 0.0285(11) 0.0343(11) 0.0070(9) 0.0036(8) 0.0052(8)
N1A 0.0186(14) 0.0144(13) 0.0192(13) -0.0004(10) 0.0005(10) -0.0008(11)
N2A 0.0178(14) 0.0136(13) 0.0203(13) 0.0011(10) 0.0001(10) -0.0014(11)
C1B 0.0257(19) 0.0198(17) 0.0223(17) 0.0007(13) 0.0031(13) -0.0034(14)
C2B 0.0191(17) 0.0168(16) 0.0286(18) 0.0022(13) 0.0063(13) 0.0002(13)
C3B 0.0174(16) 0.0166(16) 0.0216(16) 0.0025(13) 0.0008(12) -0.0027(13)
C5B 0.0148(17) 0.0205(17) 0.0281(17) 0.0001(13) 0.0029(13) -0.0018(13)
C6B 0.0173(17) 0.0251(18) 0.036(2) 0.0047(15) 0.0009(14) 0.0006(14)
C7B 0.0196(17) 0.0258(18) 0.0272(18) 0.0072(14) -0.0044(13) -0.0007(14)
C8B 0.0197(17) 0.0159(15) 0.0216(16) 0.0029(12) -0.0013(13) -0.0041(13)
C9B 0.0219(17) 0.0133(15) 0.0215(16) 0.0025(13) 0.0005(12) -0.0052(13)
C10B 0.0175(17) 0.0173(16) 0.0241(17) 0.0035(13) -0.0008(13) -0.0045(13)
C11B 0.0199(17) 0.0205(17) 0.0232(17) 0.0032(13) -0.0010(13) 0.0009(13)
C12B 0.0249(19) 0.0226(17) 0.0259(18) 0.0021(14) 0.0011(14) -0.0013(14)
C13B 0.034(2) 0.030(2) 0.0257(19) 0.0148(15) 0.0048(15) 0.0066(16)
C14B 0.044(2) 0.034(2) 0.0223(18) 0.0061(15) -0.0076(16) 0.0099(18)
C15B 0.032(2) 0.038(2) 0.0283(19) -0.0052(16) -0.0110(16) 0.0024(17)
C16B 0.0253(19) 0.0273(19) 0.0245(18) 0.0037(14) -0.0019(14) -0.0030(15)
F1B 0.0371(12) 0.0284(12) 0.0387(12) 0.0104(9) -0.0061(10) -0.0115(9)
F2B 0.0584(16) 0.0400(14) 0.0381(13) 0.0195(11) 0.0047(11) 0.0011(11)
F3B 0.0741(18) 0.0556(16) 0.0196(11) 0.0064(10) -0.0110(11) 0.0120(13)
F4B 0.0549(16) 0.0531(15) 0.0373(13) -0.0069(11) -0.0218(11) -0.0090(12)
F5B 0.0408(13) 0.0383(13) 0.0331(12) 0.0069(10) -0.0053(10) -0.0182(10)
N1B 0.0186(14) 0.0135(13) 0.0161(12) 0.0005(10) 0.0013(10) -0.0008(11)
N2B 0.0148(13) 0.0152(13) 0.0237(14) 0.0034(11) -0.0023(11) -0.0010(11)
C1C 0.0190(17) 0.0188(17) 0.0312(18) -0.0003(14) -0.0001(14) -0.0042(13)
C2C 0.0273(19) 0.0146(16) 0.0310(18) 0.0055(14) 0.0032(14) 0.0007(14)
C3C 0.0182(17) 0.0181(16) 0.0231(16) 0.0012(13) 0.0003(13) 0.0017(13)
C5C 0.0269(19) 0.0160(16) 0.0271(18) 0.0018(13) 0.0004(14) -0.0002(14)
C6C 0.031(2) 0.0215(18) 0.034(2) 0.0061(15) -0.0076(16) 0.0012(15)
C7C 0.027(2) 0.0265(19) 0.037(2) 0.0028(16) -0.0134(15) -0.0005(16)
C8C 0.0202(18) 0.0189(16) 0.0234(17) -0.0028(13) -0.0011(13) -0.0020(13)
C9C 0.0197(17) 0.0164(16) 0.0220(16) -0.0022(12) -0.0001(13) 0.0002(13)
C10C 0.0215(17) 0.0182(16) 0.0229(16) -0.0011(13) -0.0020(13) -0.0014(13)
C11C 0.0245(19) 0.0185(17) 0.0275(18) -0.0005(13) -0.0051(14) 0.0001(14)
C12C 0.026(2) 0.039(2) 0.032(2) -0.0064(17) -0.0024(15) -0.0079(16)
C13C 0.036(2) 0.033(2) 0.031(2) -0.0080(16) -0.0056(16) -0.0061(17)
C14C 0.030(2) 0.0182(17) 0.0339(19) 0.0036(15) -0.0138(15) -0.0049(15)
C15C 0.0187(18) 0.0259(19) 0.038(2) 0.0029(15) -0.0050(15) -0.0028(15)
C16C 0.0243(19) 0.0236(18) 0.0284(18) -0.0026(14) -0.0045(14) 0.0007(14)
F1C 0.0312(13) 0.090(2) 0.0461(15) -0.0289(14) 0.0095(11) -0.0200(13)
F2C 0.0452(15) 0.086(2) 0.0411(14) -0.0368(14) -0.0013(11) -0.0147(14)
F3C 0.0339(12) 0.0284(11) 0.0412(12) -0.0005(9) -0.0173(10) -0.0099(9)
F4C 0.0214(12) 0.0612(16) 0.0537(15) -0.0102(13) -0.0010(10) -0.0105(11)
F5C 0.0258(12) 0.0615(16) 0.0441(14) -0.0228(12) 0.0017(10) -0.0041(11)
N1C 0.0191(14) 0.0119(13) 0.0226(14) 0.0024(10) 0.0019(11) -0.0018(11)
N2C 0.0171(14) 0.0170(14) 0.0196(13) -0.0013(11) -0.0019(10) 0.0013(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
Ga1 N1A 2.075(3) . ?
Ga1 N2A 2.046(3) . ?
Ga1 N1B 2.057(3) . ?
Ga1 N2B 2.053(3) . ?
Ga1 N1C 2.058(3) . ?
Ga1 N2C 2.084(3) . ?
C1A H1A 0.9500 . ?
C1A C2A 1.367(5) . ?
C1A C9A 1.429(4) . ?
C2A H2A 0.9500 . ?
C2A C3A 1.411(4) . ?
C3A H3A 0.9500 . ?
C3A N1A 1.335(4) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.403(5) . ?
C5A N2A 1.336(4) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.382(5) . ?
C7A H7A 0.9500 . ?
C7A C10A 1.426(4) . ?
C8A C9A 1.394(4) . ?
C8A C10A 1.394(4) . ?
C8A C11A 1.498(4) . ?
C9A N1A 1.395(4) . ?
C10A N2A 1.395(4) . ?
C11A C12A 1.390(4) . ?
C11A C16A 1.385(4) . ?
C12A C13A 1.376(4) . ?
C12A F1A 1.343(4) . ?
C13A C14A 1.389(5) . ?
C13A F2A 1.332(4) . ?
C14A C15A 1.375(5) . ?
C14A F3A 1.338(4) . ?
C15A C16A 1.382(4) . ?
C15A F4A 1.341(3) . ?
C16A F5A 1.346(4) . ?
C1B H1B 0.9500 . ?
C1B C2B 1.372(5) . ?
C1B C9B 1.424(4) . ?
C2B H2B 0.9500 . ?
C2B C3B 1.410(4) . ?
C3B H3B 0.9500 . ?
C3B N1B 1.334(4) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.405(5) . ?
C5B N2B 1.340(4) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.371(5) . ?
C7B H7B 0.9500 . ?
C7B C10B 1.426(5) . ?
C8B C9B 1.387(4) . ?
C8B C10B 1.396(5) . ?
C8B C11B 1.501(4) . ?
C9B N1B 1.398(4) . ?
C10B N2B 1.393(4) . ?
C11B C12B 1.391(5) . ?
C11B C16B 1.376(5) . ?
C12B C13B 1.386(5) . ?
C12B F1B 1.341(4) . ?
C13B C14B 1.372(5) . ?
C13B F2B 1.343(4) . ?
C14B C15B 1.373(6) . ?
C14B F3B 1.333(4) . ?
C15B C16B 1.382(5) . ?
C15B F4B 1.340(4) . ?
C16B F5B 1.343(4) . ?
C1C H1C 0.9500 . ?
C1C C2C 1.373(5) . ?
C1C C9C 1.421(4) . ?
C2C H2C 0.9500 . ?
C2C C3C 1.404(5) . ?
C3C H3C 0.9500 . ?
C3C N1C 1.339(4) . ?
C5C H5C 0.9500 . ?
C5C C6C 1.406(5) . ?
C5C N2C 1.341(4) . ?
C6C H6C 0.9500 . ?
C6C C7C 1.379(5) . ?
C7C H7C 0.9500 . ?
C7C C10C 1.422(5) . ?
C8C C9C 1.398(4) . ?
C8C C10C 1.384(5) . ?
C8C C11C 1.506(4) . ?
C9C N1C 1.393(4) . ?
C10C N2C 1.400(4) . ?
C11C C12C 1.383(5) . ?
C11C C16C 1.379(5) . ?
C12C C13C 1.386(5) . ?
C12C F1C 1.339(4) . ?
C13C C14C 1.364(5) . ?
C13C F2C 1.343(4) . ?
C14C C15C 1.370(5) . ?
C14C F3C 1.338(4) . ?
C15C C16C 1.389(5) . ?
C15C F4C 1.328(4) . ?
C16C F5C 1.341(4) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1A Ga1 N2C 86.70(10) . . ?
N2A Ga1 N1A 88.72(10) . . ?
N2A Ga1 N1B 91.76(10) . . ?
N2A Ga1 N2B 91.73(10) . . ?
N2A Ga1 N1C 176.82(10) . . ?
N2A Ga1 N2C 89.28(10) . . ?
N1B Ga1 N1A 178.60(10) . . ?
N1B Ga1 N1C 90.42(10) . . ?
N1B Ga1 N2C 92.00(10) . . ?
N2B Ga1 N1A 92.35(10) . . ?
N2B Ga1 N1B 88.95(10) . . ?
N2B Ga1 N1C 90.62(10) . . ?
N2B Ga1 N2C 178.60(11) . . ?
N1C Ga1 N1A 89.05(10) . . ?
N1C Ga1 N2C 88.33(10) . . ?
C2A C1A H1A 126.6 . . ?
C2A C1A C9A 106.9(3) . . ?
C9A C1A H1A 126.6 . . ?
C1A C2A H2A 126.6 . . ?
C1A C2A C3A 106.9(3) . . ?
C3A C2A H2A 126.6 . . ?
C2A C3A H3A 124.5 . . ?
N1A C3A C2A 111.1(3) . . ?
N1A C3A H3A 124.5 . . ?
C6A C5A H5A 124.1 . . ?
N2A C5A H5A 124.1 . . ?
N2A C5A C6A 111.7(3) . . ?
C5A C6A H6A 126.8 . . ?
C7A C6A C5A 106.4(3) . . ?
C7A C6A H6A 126.8 . . ?
C6A C7A H7A 126.6 . . ?
C6A C7A C10A 106.8(3) . . ?
C10A C7A H7A 126.6 . . ?
C9A C8A C10A 127.2(3) . . ?
C9A C8A C11A 116.4(3) . . ?
C10A C8A C11A 116.4(3) . . ?
C8A C9A C1A 127.2(3) . . ?
C8A C9A N1A 124.4(3) . . ?
N1A C9A C1A 108.3(3) . . ?
C8A C10A C7A 127.5(3) . . ?
C8A C10A N2A 124.1(3) . . ?
N2A C10A C7A 108.5(3) . . ?
C12A C11A C8A 122.4(3) . . ?
C16A C11A C8A 121.3(3) . . ?
C16A C11A C12A 116.3(3) . . ?
C13A C12A C11A 122.8(3) . . ?
F1A C12A C11A 119.2(3) . . ?
F1A C12A C13A 117.9(3) . . ?
C12A C13A C14A 118.9(3) . . ?
F2A C13A C12A 120.9(3) . . ?
F2A C13A C14A 120.2(3) . . ?
C15A C14A C13A 119.9(3) . . ?
F3A C14A C13A 119.7(3) . . ?
F3A C14A C15A 120.3(3) . . ?
C14A C15A C16A 119.6(3) . . ?
F4A C15A C14A 119.7(3) . . ?
F4A C15A C16A 120.6(3) . . ?
C15A C16A C11A 122.3(3) . . ?
F5A C16A C11A 120.0(3) . . ?
F5A C16A C15A 117.7(3) . . ?
C3A N1A Ga1 126.5(2) . . ?
C3A N1A C9A 106.8(3) . . ?
C9A N1A Ga1 124.9(2) . . ?
C5A N2A Ga1 126.1(2) . . ?
C5A N2A C10A 106.6(3) . . ?
C10A N2A Ga1 126.8(2) . . ?
C2B C1B H1B 126.6 . . ?
C2B C1B C9B 106.9(3) . . ?
C9B C1B H1B 126.6 . . ?
C1B C2B H2B 126.7 . . ?
C1B C2B C3B 106.6(3) . . ?
C3B C2B H2B 126.7 . . ?
C2B C3B H3B 124.3 . . ?
N1B C3B C2B 111.4(3) . . ?
N1B C3B H3B 124.3 . . ?
C6B C5B H5B 124.0 . . ?
N2B C5B H5B 124.0 . . ?
N2B C5B C6B 112.0(3) . . ?
C5B C6B H6B 126.9 . . ?
C7B C6B C5B 106.1(3) . . ?
C7B C6B H6B 126.9 . . ?
C6B C7B H7B 126.4 . . ?
C6B C7B C10B 107.2(3) . . ?
C10B C7B H7B 126.4 . . ?
C9B C8B C10B 127.6(3) . . ?
C9B C8B C11B 116.7(3) . . ?
C10B C8B C11B 115.7(3) . . ?
C8B C9B C1B 127.6(3) . . ?
C8B C9B N1B 123.8(3) . . ?
N1B C9B C1B 108.5(3) . . ?
C8B C10B C7B 127.3(3) . . ?
N2B C10B C7B 108.6(3) . . ?
N2B C10B C8B 124.1(3) . . ?
C12B C11B C8B 121.2(3) . . ?
C16B C11B C8B 122.2(3) . . ?
C16B C11B C12B 116.5(3) . . ?
C13B C12B C11B 121.7(3) . . ?
F1B C12B C11B 119.6(3) . . ?
F1B C12B C13B 118.7(3) . . ?
C14B C13B C12B 120.0(3) . . ?
F2B C13B C12B 119.6(3) . . ?
F2B C13B C14B 120.5(3) . . ?
C13B C14B C15B 119.6(3) . . ?
F3B C14B C13B 119.7(3) . . ?
F3B C14B C15B 120.7(4) . . ?
C14B C15B C16B 119.7(3) . . ?
F4B C15B C14B 120.0(3) . . ?
F4B C15B C16B 120.3(4) . . ?
C11B C16B C15B 122.6(3) . . ?
F5B C16B C11B 119.8(3) . . ?
F5B C16B C15B 117.7(3) . . ?
C3B N1B Ga1 126.0(2) . . ?
C3B N1B C9B 106.5(3) . . ?
C9B N1B Ga1 127.5(2) . . ?
C5B N2B Ga1 126.1(2) . . ?
C5B N2B C10B 106.1(3) . . ?
C10B N2B Ga1 127.0(2) . . ?
C2C C1C H1C 126.7 . . ?
C2C C1C C9C 106.7(3) . . ?
C9C C1C H1C 126.7 . . ?
C1C C2C H2C 126.5 . . ?
C1C C2C C3C 106.9(3) . . ?
C3C C2C H2C 126.5 . . ?
C2C C3C H3C 124.4 . . ?
N1C C3C C2C 111.1(3) . . ?
N1C C3C H3C 124.4 . . ?
C6C C5C H5C 124.2 . . ?
N2C C5C H5C 124.2 . . ?
N2C C5C C6C 111.6(3) . . ?
C5C C6C H6C 126.7 . . ?
C7C C6C C5C 106.6(3) . . ?
C7C C6C H6C 126.7 . . ?
C6C C7C H7C 126.6 . . ?
C6C C7C C10C 106.9(3) . . ?
C10C C7C H7C 126.6 . . ?
C9C C8C C11C 115.1(3) . . ?
C10C C8C C9C 128.2(3) . . ?
C10C C8C C11C 116.7(3) . . ?
C8C C9C C1C 127.6(3) . . ?
N1C C9C C1C 108.7(3) . . ?
N1C C9C C8C 123.7(3) . . ?
C8C C10C C7C 127.5(3) . . ?
C8C C10C N2C 123.7(3) . . ?
N2C C10C C7C 108.7(3) . . ?
C12C C11C C8C 121.0(3) . . ?
C16C C11C C8C 122.4(3) . . ?
C16C C11C C12C 116.6(3) . . ?
C11C C12C C13C 122.0(4) . . ?
F1C C12C C11C 119.5(3) . . ?
F1C C12C C13C 118.5(3) . . ?
C14C C13C C12C 119.7(4) . . ?
F2C C13C C12C 119.9(4) . . ?
F2C C13C C14C 120.4(3) . . ?
C13C C14C C15C 120.2(3) . . ?
F3C C14C C13C 119.9(3) . . ?
F3C C14C C15C 119.8(3) . . ?
C14C C15C C16C 119.2(3) . . ?
F4C C15C C14C 120.2(3) . . ?
F4C C15C C16C 120.6(3) . . ?
C11C C16C C15C 122.3(3) . . ?
F5C C16C C11C 119.5(3) . . ?
F5C C16C C15C 118.2(3) . . ?
C3C N1C Ga1 126.2(2) . . ?
C3C N1C C9C 106.5(3) . . ?
C9C N1C Ga1 126.8(2) . . ?
C5C N2C Ga1 126.8(2) . . ?
C5C N2C C10C 106.3(3) . . ?
C10C N2C Ga1 125.4(2) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1A H1A F3C 0.95 2.55 3.479(4) 166.6 3_655
C7A H7A F1A 0.95 2.46 3.403(4) 173.0 8_765
C3B H3B N2C 0.95 2.60 3.086(4) 111.8 .
C5B H5B N1A 0.95 2.62 3.090(4) 110.9 .
C7B H7B F5B 0.95 2.44 3.237(4) 141.9 8_755
C7C H7C F4A 0.95 2.55 3.497(4) 174.0 3_645
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
C1A C2A C3A N1A 0.2(4) . . . . ?
C1A C9A N1A Ga1 -165.5(2) . . . . ?
C1A C9A N1A C3A 0.4(4) . . . . ?
C2A C1A C9A C8A 176.6(3) . . . . ?
C2A C1A C9A N1A -0.3(4) . . . . ?
C2A C3A N1A Ga1 165.3(2) . . . . ?
C2A C3A N1A C9A -0.3(4) . . . . ?
C5A C6A C7A C10A -0.6(4) . . . . ?
C6A C5A N2A Ga1 -173.3(2) . . . . ?
C6A C5A N2A C10A -0.5(4) . . . . ?
C6A C7A C10A C8A -179.5(3) . . . . ?
C6A C7A C10A N2A 0.3(4) . . . . ?
C7A C10A N2A Ga1 172.9(2) . . . . ?
C7A C10A N2A C5A 0.1(3) . . . . ?
C8A C9A N1A Ga1 17.5(4) . . . . ?
C8A C9A N1A C3A -176.6(3) . . . . ?
C8A C10A N2A Ga1 -7.2(4) . . . . ?
C8A C10A N2A C5A -180.0(3) . . . . ?
C8A C11A C12A C13A 178.9(3) . . . . ?
C8A C11A C12A F1A 0.1(5) . . . . ?
C8A C11A C16A C15A -178.7(3) . . . . ?
C8A C11A C16A F5A 0.2(5) . . . . ?
C9A C1A C2A C3A 0.1(4) . . . . ?
C9A C8A C10A C7A 174.7(3) . . . . ?
C9A C8A C10A N2A -5.1(5) . . . . ?
C9A C8A C11A C12A -73.8(4) . . . . ?
C9A C8A C11A C16A 105.5(4) . . . . ?
C10A C8A C9A C1A -177.0(3) . . . . ?
C10A C8A C9A N1A -0.6(5) . . . . ?
C10A C8A C11A C12A 106.1(4) . . . . ?
C10A C8A C11A C16A -74.7(4) . . . . ?
C11A C8A C9A C1A 2.9(5) . . . . ?
C11A C8A C9A N1A 179.3(3) . . . . ?
C11A C8A C10A C7A -5.1(5) . . . . ?
C11A C8A C10A N2A 175.0(3) . . . . ?
C11A C12A C13A C14A 0.2(5) . . . . ?
C11A C12A C13A F2A -179.2(3) . . . . ?
C12A C11A C16A C15A 0.6(5) . . . . ?
C12A C11A C16A F5A 179.5(3) . . . . ?
C12A C13A C14A C15A -0.4(5) . . . . ?
C12A C13A C14A F3A -178.6(3) . . . . ?
C13A C14A C15A C16A 0.7(5) . . . . ?
C13A C14A C15A F4A -178.7(3) . . . . ?
C14A C15A C16A C11A -0.8(5) . . . . ?
C14A C15A C16A F5A -179.7(3) . . . . ?
C16A C11A C12A C13A -0.3(5) . . . . ?
C16A C11A C12A F1A -179.2(3) . . . . ?
F1A C12A C13A C14A 179.1(3) . . . . ?
F1A C12A C13A F2A -0.3(5) . . . . ?
F2A C13A C14A C15A 179.0(3) . . . . ?
F2A C13A C14A F3A 0.8(5) . . . . ?
F3A C14A C15A C16A 178.8(3) . . . . ?
F3A C14A C15A F4A -0.5(5) . . . . ?
F4A C15A C16A C11A 178.5(3) . . . . ?
F4A C15A C16A F5A -0.4(5) . . . . ?
N2A C5A C6A C7A 0.8(4) . . . . ?
C1B C2B C3B N1B -1.2(4) . . . . ?
C1B C9B N1B Ga1 179.1(2) . . . . ?
C1B C9B N1B C3B -0.4(3) . . . . ?
C2B C1B C9B C8B -179.8(3) . . . . ?
C2B C1B C9B N1B -0.3(4) . . . . ?
C2B C3B N1B Ga1 -178.6(2) . . . . ?
C2B C3B N1B C9B 1.0(3) . . . . ?
C5B C6B C7B C10B 0.3(4) . . . . ?
C6B C5B N2B Ga1 -168.5(2) . . . . ?
C6B C5B N2B C10B 1.3(4) . . . . ?
C6B C7B C10B C8B 180.0(3) . . . . ?
C6B C7B C10B N2B 0.5(4) . . . . ?
C7B C10B N2B Ga1 168.6(2) . . . . ?
C7B C10B N2B C5B -1.1(3) . . . . ?
C8B C9B N1B Ga1 -1.3(4) . . . . ?
C8B C9B N1B C3B 179.2(3) . . . . ?
C8B C10B N2B Ga1 -10.9(4) . . . . ?
C8B C10B N2B C5B 179.4(3) . . . . ?
C8B C11B C12B C13B 177.6(3) . . . . ?
C8B C11B C12B F1B -1.6(5) . . . . ?
C8B C11B C16B C15B -177.4(3) . . . . ?
C8B C11B C16B F5B 3.3(5) . . . . ?
C9B C1B C2B C3B 0.9(4) . . . . ?
C9B C8B C10B C7B -178.4(3) . . . . ?
C9B C8B C10B N2B 1.0(5) . . . . ?
C9B C8B C11B C12B 86.5(4) . . . . ?
C9B C8B C11B C16B -95.7(4) . . . . ?
C10B C8B C9B C1B -175.1(3) . . . . ?
C10B C8B C9B N1B 5.5(5) . . . . ?
C10B C8B C11B C12B -92.8(4) . . . . ?
C10B C8B C11B C16B 85.0(4) . . . . ?
C11B C8B C9B C1B 5.7(5) . . . . ?
C11B C8B C9B N1B -173.7(3) . . . . ?
C11B C8B C10B C7B 0.8(5) . . . . ?
C11B C8B C10B N2B -179.8(3) . . . . ?
C11B C12B C13B C14B 0.1(6) . . . . ?
C11B C12B C13B F2B -179.5(3) . . . . ?
C12B C11B C16B C15B 0.4(5) . . . . ?
C12B C11B C16B F5B -178.9(3) . . . . ?
C12B C13B C14B C15B 0.1(6) . . . . ?
C12B C13B C14B F3B 179.7(3) . . . . ?
C13B C14B C15B C16B 0.0(6) . . . . ?
C13B C14B C15B F4B 178.3(3) . . . . ?
C14B C15B C16B C11B -0.3(6) . . . . ?
C14B C15B C16B F5B 179.0(3) . . . . ?
C16B C11B C12B C13B -0.3(5) . . . . ?
C16B C11B C12B F1B -179.5(3) . . . . ?
F1B C12B C13B C14B 179.3(3) . . . . ?
F1B C12B C13B F2B -0.3(5) . . . . ?
F2B C13B C14B C15B 179.7(3) . . . . ?
F2B C13B C14B F3B -0.8(6) . . . . ?
F3B C14B C15B C16B -179.6(3) . . . . ?
F3B C14B C15B F4B -1.3(6) . . . . ?
F4B C15B C16B C11B -178.6(3) . . . . ?
F4B C15B C16B F5B 0.7(5) . . . . ?
N2B C5B C6B C7B -1.1(4) . . . . ?
C1C C2C C3C N1C 1.3(4) . . . . ?
C1C C9C N1C Ga1 172.3(2) . . . . ?
C1C C9C N1C C3C 0.5(4) . . . . ?
C2C C1C C9C C8C -179.2(3) . . . . ?
C2C C1C C9C N1C 0.3(4) . . . . ?
C2C C3C N1C Ga1 -172.9(2) . . . . ?
C2C C3C N1C C9C -1.0(4) . . . . ?
C5C C6C C7C C10C 0.0(4) . . . . ?
C6C C5C N2C Ga1 166.4(2) . . . . ?
C6C C5C N2C C10C 0.3(4) . . . . ?
C6C C7C C10C C8C 177.4(4) . . . . ?
C6C C7C C10C N2C 0.2(4) . . . . ?
C7C C10C N2C Ga1 -166.6(2) . . . . ?
C7C C10C N2C C5C -0.3(4) . . . . ?
C8C C9C N1C Ga1 -8.2(4) . . . . ?
C8C C9C N1C C3C 180.0(3) . . . . ?
C8C C10C N2C Ga1 16.0(4) . . . . ?
C8C C10C N2C C5C -177.7(3) . . . . ?
C8C C11C C12C C13C 176.9(3) . . . . ?
C8C C11C C12C F1C -3.0(6) . . . . ?
C8C C11C C16C C15C -177.6(3) . . . . ?
C8C C11C C16C F5C 1.7(5) . . . . ?
C9C C1C C2C C3C -0.9(4) . . . . ?
C9C C8C C10C C7C -175.5(4) . . . . ?
C9C C8C C10C N2C 1.3(6) . . . . ?
C9C C8C C11C C12C -92.5(4) . . . . ?
C9C C8C C11C C16C 84.1(4) . . . . ?
C10C C8C C9C C1C 173.7(3) . . . . ?
C10C C8C C9C N1C -5.7(5) . . . . ?
C10C C8C C11C C12C 86.8(4) . . . . ?
C10C C8C C11C C16C -96.5(4) . . . . ?
C11C C8C C9C C1C -7.0(5) . . . . ?
C11C C8C C9C N1C 173.6(3) . . . . ?
C11C C8C C10C C7C 5.2(5) . . . . ?
C11C C8C C10C N2C -177.9(3) . . . . ?
C11C C12C C13C C14C 0.0(6) . . . . ?
C11C C12C C13C F2C 179.6(4) . . . . ?
C12C C11C C16C C15C -0.8(5) . . . . ?
C12C C11C C16C F5C 178.5(3) . . . . ?
C12C C13C C14C C15C 0.6(6) . . . . ?
C12C C13C C14C F3C -178.8(3) . . . . ?
C13C C14C C15C C16C -1.4(5) . . . . ?
C13C C14C C15C F4C -178.4(3) . . . . ?
C14C C15C C16C C11C 1.5(5) . . . . ?
C14C C15C C16C F5C -177.8(3) . . . . ?
C16C C11C C12C C13C 0.1(6) . . . . ?
C16C C11C C12C F1C -179.9(3) . . . . ?
F1C C12C C13C C14C 180.0(4) . . . . ?
F1C C12C C13C F2C -0.5(6) . . . . ?
F2C C13C C14C C15C -178.9(4) . . . . ?
F2C C13C C14C F3C 1.6(6) . . . . ?
F3C C14C C15C C16C 178.1(3) . . . . ?
F3C C14C C15C F4C 1.1(5) . . . . ?
F4C C15C C16C C11C 178.5(3) . . . . ?
F4C C15C C16C F5C -0.9(5) . . . . ?
N2C C5C C6C C7C -0.2(4) . . . . ?
_shelx_res_file
;
kjf138_a.res created by SHELXL-2014/7
TITL kjf138_a.res in Pbca
REM Old TITL kjf138 in Pbca
REM SHELXT solution in Pbca
REM R1 0.111, Rweak 0.005, Alpha 0.031, Orientation as input
REM Formula found by SHELXT: C45 N6 F15 Ga
CELL 1.54178 25.765 8.8371 35.7783 90 90 90
ZERR 8 0.0008 0.0003 0.0011 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H F Ga N
UNIT 360 144 120 8 48
EQIV $1 1-X,0.5+Y,0.5-Z
EQIV $2 1.5-X,-0.5+Y,+Z
EQIV $3 1.5-X,0.5+Y,+Z
EQIV $4 1-X,-0.5+Y,0.5-Z
L.S. 10
PLAN 20
SIZE 0.09 0.16 0.37
TEMP -173(2)
HTAB C3B N2C
HTAB C5B N1A
HTAB C1A F3C_$1
HTAB C7B F5B_$2
HTAB C7A F1A_$3
HTAB C7C F4A_$4
BOND $H
HTAB
WPDB
MORE -1
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.053200 11.715800
FVAR 0.18890
GA1 4 0.599988 0.458534 0.409087 11.00000 0.01668 0.01241 =
0.01817 0.00116 0.00031 -0.00086
C1A 1 0.647434 0.354139 0.297113 11.00000 0.02191 0.01855 =
0.02129 -0.00033 0.00074 0.00209
AFIX 43
H1A 2 0.658092 0.381370 0.272600 11.00000 -1.20000
AFIX 0
C2A 1 0.631787 0.213970 0.308743 11.00000 0.02407 0.01768 =
0.02737 -0.00431 0.00210 -0.00075
AFIX 43
H2A 2 0.629529 0.125181 0.293862 11.00000 -1.20000
AFIX 0
C3A 1 0.619637 0.226446 0.347071 11.00000 0.02217 0.01302 =
0.02686 0.00389 0.00073 0.00036
AFIX 43
H3A 2 0.607769 0.145144 0.362194 11.00000 -1.20000
AFIX 0
C5A 1 0.645361 0.772281 0.419629 11.00000 0.02046 0.01817 =
0.02160 -0.00159 -0.00005 0.00132
AFIX 43
H5A 2 0.634935 0.773713 0.445095 11.00000 -1.20000
AFIX 0
C6A 1 0.669144 0.894368 0.401309 11.00000 0.02297 0.01548 =
0.03059 -0.00121 -0.00149 -0.00236
AFIX 43
H6A 2 0.677796 0.989748 0.411855 11.00000 -1.20000
AFIX 0
C7A 1 0.677485 0.848348 0.364885 11.00000 0.01793 0.01571 =
0.02897 0.00716 0.00311 -0.00052
AFIX 43
H7A 2 0.692725 0.906457 0.345427 11.00000 -1.20000
AFIX 0
C8A 1 0.659371 0.603443 0.330730 11.00000 0.01477 0.01614 =
0.02292 0.00397 -0.00066 0.00182
C9A 1 0.644689 0.451819 0.328879 11.00000 0.01780 0.01596 =
0.02086 0.00103 0.00097 0.00308
C10A 1 0.658814 0.696857 0.362128 11.00000 0.01683 0.01814 =
0.02152 0.00254 0.00078 0.00077
C11A 1 0.677934 0.673736 0.295059 11.00000 0.01943 0.01347 =
0.02103 0.00016 -0.00044 -0.00204
C12A 1 0.726280 0.641314 0.279808 11.00000 0.02270 0.01539 =
0.01814 0.00023 -0.00192 -0.00040
C13A 1 0.743389 0.703357 0.246761 11.00000 0.01865 0.01845 =
0.02239 -0.00210 0.00175 -0.00161
C14A 1 0.711228 0.803214 0.227705 11.00000 0.02613 0.01831 =
0.01664 0.00199 0.00069 -0.00650
C15A 1 0.663061 0.837796 0.241853 11.00000 0.02353 0.01511 =
0.02311 0.00618 -0.00642 0.00082
C16A 1 0.647176 0.773987 0.275196 11.00000 0.01753 0.01476 =
0.02784 0.00137 0.00092 0.00118
F1A 3 0.757709 0.543488 0.297472 11.00000 0.02148 0.02327 =
0.02572 0.00625 -0.00004 0.00576
F2A 3 0.789777 0.667766 0.232893 11.00000 0.02497 0.02551 =
0.02531 -0.00040 0.00686 -0.00033
F3A 3 0.726800 0.862044 0.195134 11.00000 0.03633 0.02948 =
0.02044 0.00796 0.00250 -0.00319
F4A 3 0.631757 0.931894 0.222992 11.00000 0.02858 0.02635 =
0.03257 0.01198 -0.00748 0.00258
F5A 3 0.599647 0.810417 0.287928 11.00000 0.02115 0.02850 =
0.03431 0.00699 0.00357 0.00524
N1A 5 0.627020 0.367593 0.359285 11.00000 0.01861 0.01445 =
0.01920 -0.00040 0.00049 -0.00077
N2A 5 0.639177 0.653803 0.396875 11.00000 0.01782 0.01361 =
0.02033 0.00110 0.00011 -0.00141
C1B 1 0.559808 0.614889 0.519260 11.00000 0.02569 0.01983 =
0.02226 0.00073 0.00314 -0.00337
AFIX 43
H1B 2 0.564300 0.622381 0.545550 11.00000 -1.20000
AFIX 0
C2B 1 0.521780 0.683093 0.498383 11.00000 0.01910 0.01680 =
0.02861 0.00221 0.00635 0.00019
AFIX 43
H2B 2 0.495133 0.747917 0.507352 11.00000 -1.20000
AFIX 0
C3B 1 0.529929 0.638281 0.461023 11.00000 0.01736 0.01664 =
0.02163 0.00253 0.00078 -0.00270
AFIX 43
H3B 2 0.508590 0.668007 0.440652 11.00000 -1.20000
AFIX 0
C5B 1 0.700958 0.291750 0.424661 11.00000 0.01482 0.02048 =
0.02810 0.00007 0.00286 -0.00184
AFIX 43
H5B 2 0.707082 0.277869 0.398703 11.00000 -1.20000
AFIX 0
C6B 1 0.731693 0.227701 0.452984 11.00000 0.01731 0.02509 =
0.03608 0.00466 0.00088 0.00064
AFIX 43
H6B 2 0.760972 0.163652 0.449793 11.00000 -1.20000
AFIX 0
C7B 1 0.710910 0.276270 0.486149 11.00000 0.01961 0.02583 =
0.02722 0.00724 -0.00445 -0.00072
AFIX 43
H7B 2 0.723235 0.252484 0.510474 11.00000 -1.20000
AFIX 0
C8B 1 0.634365 0.442993 0.502361 11.00000 0.01974 0.01595 =
0.02161 0.00292 -0.00133 -0.00415
C9B 1 0.591273 0.530692 0.493990 11.00000 0.02186 0.01333 =
0.02147 0.00248 0.00048 -0.00518
C10B 1 0.667337 0.369161 0.477331 11.00000 0.01750 0.01735 =
0.02414 0.00347 -0.00076 -0.00446
C11B 1 0.646994 0.422915 0.543014 11.00000 0.01992 0.02054 =
0.02323 0.00320 -0.00096 0.00095
C12B 1 0.624242 0.308239 0.564021 11.00000 0.02490 0.02262 =
0.02594 0.00210 0.00111 -0.00128
C13B 1 0.637054 0.285144 0.601201 11.00000 0.03413 0.03026 =
0.02570 0.01483 0.00480 0.00664
C14B 1 0.672965 0.376762 0.618200 11.00000 0.04406 0.03361 =
0.02231 0.00614 -0.00756 0.00986
C15B 1 0.695965 0.491128 0.598165 11.00000 0.03158 0.03797 =
0.02829 -0.00517 -0.01099 0.00243
C16B 1 0.682669 0.512634 0.561133 11.00000 0.02527 0.02733 =
0.02447 0.00373 -0.00190 -0.00298
F1B 3 0.589452 0.215877 0.548023 11.00000 0.03705 0.02841 =
0.03869 0.01037 -0.00613 -0.01146
F2B 3 0.614351 0.172269 0.620276 11.00000 0.05838 0.04003 =
0.03810 0.01948 0.00471 0.00112
F3B 3 0.684961 0.354612 0.654016 11.00000 0.07406 0.05562 =
0.01957 0.00645 -0.01101 0.01204
F4B 3 0.730109 0.583605 0.614789 11.00000 0.05486 0.05312 =
0.03726 -0.00690 -0.02184 -0.00896
F5B 3 0.705518 0.627175 0.542768 11.00000 0.04079 0.03832 =
0.03306 0.00685 -0.00529 -0.01824
N1B 5 0.571397 0.548866 0.457914 11.00000 0.01861 0.01346 =
0.01609 0.00048 0.00134 -0.00084
N2B 5 0.661990 0.374720 0.438616 11.00000 0.01479 0.01516 =
0.02369 0.00337 -0.00229 -0.00097
C1C 1 0.503742 0.062210 0.410567 11.00000 0.01902 0.01883 =
0.03121 -0.00027 -0.00009 -0.00421
AFIX 43
H1C 2 0.476207 0.000412 0.401687 11.00000 -1.20000
AFIX 0
C2C 1 0.539560 0.024633 0.437404 11.00000 0.02728 0.01464 =
0.03102 0.00555 0.00321 0.00073
AFIX 43
H2C 2 0.541289 -0.067774 0.450915 11.00000 -1.20000
AFIX 0
C3C 1 0.573150 0.148807 0.441077 11.00000 0.01822 0.01806 =
0.02310 0.00119 0.00026 0.00167
AFIX 43
H3C 2 0.602065 0.152083 0.457533 11.00000 -1.20000
AFIX 0
C5C 1 0.531628 0.676336 0.363345 11.00000 0.02687 0.01599 =
0.02715 0.00181 0.00043 -0.00021
AFIX 43
H5C 2 0.553170 0.760309 0.369192 11.00000 -1.20000
AFIX 0
C6C 1 0.490294 0.681172 0.337708 11.00000 0.03147 0.02147 =
0.03395 0.00614 -0.00757 0.00120
AFIX 43
H6C 2 0.479187 0.766401 0.323641 11.00000 -1.20000
AFIX 0
C7C 1 0.469042 0.538036 0.336982 11.00000 0.02693 0.02645 =
0.03668 0.00282 -0.01342 -0.00045
AFIX 43
H7C 2 0.440419 0.505595 0.322286 11.00000 -1.20000
AFIX 0
C8C 1 0.489714 0.298488 0.371966 11.00000 0.02016 0.01886 =
0.02336 -0.00277 -0.00105 -0.00205
C9C 1 0.515835 0.211471 0.398641 11.00000 0.01972 0.01637 =
0.02197 -0.00220 -0.00015 0.00017
C10C 1 0.498165 0.448225 0.362442 11.00000 0.02153 0.01817 =
0.02290 -0.00107 -0.00204 -0.00143
C11C 1 0.447582 0.216815 0.350913 11.00000 0.02454 0.01855 =
0.02749 -0.00054 -0.00508 0.00006
C12C 1 0.457884 0.145951 0.317251 11.00000 0.02591 0.03858 =
0.03235 -0.00639 -0.00241 -0.00790
C13C 1 0.420337 0.064045 0.298266 11.00000 0.03561 0.03310 =
0.03103 -0.00799 -0.00561 -0.00606
C14C 1 0.371604 0.051999 0.312838 11.00000 0.03039 0.01825 =
0.03394 0.00356 -0.01378 -0.00489
C15C 1 0.359584 0.121715 0.345920 11.00000 0.01871 0.02587 =
0.03758 0.00289 -0.00503 -0.00277
C16C 1 0.397900 0.201817 0.364743 11.00000 0.02435 0.02362 =
0.02839 -0.00263 -0.00447 0.00070
F1C 3 0.505428 0.155896 0.302338 11.00000 0.03119 0.08997 =
0.04611 -0.02891 0.00954 -0.02002
F2C 3 0.431990 -0.002063 0.265537 11.00000 0.04523 0.08628 =
0.04114 -0.03685 -0.00129 -0.01466
F3C 3 0.335483 -0.029178 0.294931 11.00000 0.03389 0.02840 =
0.04123 -0.00053 -0.01731 -0.00993
F4C 3 0.312497 0.106907 0.360544 11.00000 0.02141 0.06119 =
0.05374 -0.01021 -0.00098 -0.01053
F5C 3 0.385726 0.264962 0.397677 11.00000 0.02582 0.06145 =
0.04414 -0.02282 0.00165 -0.00413
N1C 5 0.559111 0.262026 0.418359 11.00000 0.01905 0.01186 =
0.02262 0.00242 0.00188 -0.00178
N2C 5 0.536844 0.538410 0.378508 11.00000 0.01714 0.01696 =
0.01961 -0.00128 -0.00191 0.00126
HKLF 4
REM kjf138_a.res in Pbca
REM R1 = 0.0477 for 5728 Fo > 4sig(Fo) and 0.0679 for all 7436 data
REM 604 parameters refined using 0 restraints
END
WGHT 0.0532 11.7272
REM Instructions for potential hydrogen bonds
HTAB C1A F3C_$1
HTAB C7A F1A_$3
EQIV $5 -x+1, -y+1, -z+1
HTAB C1B F5C_$5
HTAB C3B N2C
HTAB C5B N1A
HTAB C7B F5B_$2
HTAB C7C F4A_$4
REM Highest difference peak 0.587, deepest hole -0.443, 1-sigma level 0.080
Q1 1 0.5942 0.3406 0.4084 11.00000 0.05 0.59
Q2 1 0.6108 0.5828 0.4062 11.00000 0.05 0.57
Q3 1 0.6184 0.4619 0.4347 11.00000 0.05 0.47
Q4 1 0.6101 0.4470 0.3790 11.00000 0.05 0.46
Q5 1 0.5719 0.4742 0.3875 11.00000 0.05 0.46
Q6 1 0.5630 0.5032 0.3924 11.00000 0.05 0.45
Q7 1 0.6325 0.4434 0.4309 11.00000 0.05 0.44
Q8 1 0.5987 0.7053 0.3969 11.00000 0.05 0.39
Q9 1 0.6576 0.4140 0.3651 11.00000 0.05 0.38
Q10 1 0.6538 0.6457 0.4218 11.00000 0.05 0.35
Q11 1 0.5726 0.5368 0.4236 11.00000 0.05 0.34
Q12 1 0.6396 0.5707 0.6578 11.00000 0.05 0.33
Q13 1 0.5629 0.5719 0.3601 11.00000 0.05 0.32
Q14 1 0.5991 0.5228 0.4706 11.00000 0.05 0.32
Q15 1 0.5806 0.5129 0.4350 11.00000 0.05 0.32
Q16 1 0.5704 0.6445 0.4526 11.00000 0.05 0.32
Q17 1 0.5546 0.5909 0.3651 11.00000 0.05 0.31
Q18 1 0.6027 0.0333 0.2715 11.00000 0.05 0.31
Q19 1 0.5707 0.2601 0.4427 11.00000 0.05 0.31
Q20 1 0.5972 0.2180 0.4201 11.00000 0.05 0.30
;
_shelx_res_checksum 23399
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN micromount using oil'
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT601_kjf138_a
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 56 Ang**3
RESPONSE: Highest residual density peaks are centred on the core metal.
This results in no sufficient density to model a solvent within the solvent
accessible void.
;
_vrf_PLAT906_kjf138_a
;
PROBLEM: Large K Value in the Analysis of Variance ...... 2.179 Check
RESPONSE: Due to weak high angle data.
;
_vrf_PLAT911_kjf138_a
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 25 Report
RESPONSE: Data collected to 99.5 % completeness resulting in missing
reflections.
;
_vrf_PLAT978_kjf138_a
;
PROBLEM: Number C-C Bonds with Positive Residual Density. 0 Info
RESPONSE: Due to weak high angle data.
;
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_kjf141
_database_code_depnum_ccdc_archive 'CCDC 1841035'
_audit_update_record
;
2018-05-02 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;
_audit_creation_date 2018-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic
{Tris[5-(4-butyloxytetrafluorophenyl)dipyrrin]}-gallium(III)
_chemical_formula_moiety 'C57 H45 F12 Ga1 N6 O3'
_chemical_formula_sum 'C57 H45 F12 Ga N6 O3'
_chemical_formula_weight 1159.71
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system trigonal
_space_group_IT_number 148
_space_group_name_H-M_alt 'R -3'
_space_group_name_Hall '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
_cell_length_a 24.0883(10)
_cell_length_b 24.0883(10)
_cell_length_c 15.2527(7)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 7664.6(7)
_cell_formula_units_Z 6
_cell_measurement_reflns_used 9857
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 30.84
_cell_measurement_theta_min 2.37
_shelx_estimated_absorpt_T_max 0.951
_shelx_estimated_absorpt_T_min 0.742
_exptl_absorpt_coefficient_mu 0.635
_exptl_absorpt_correction_T_max 0.7462
_exptl_absorpt_correction_T_min 0.6857
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0602 before and 0.0451 after correction. The Ratio of minimum to maximum transmission is 0.9189. The \l/2 correction factor is 0.00150.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light orange'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.508
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Needle
_exptl_crystal_F_000 3552
_exptl_crystal_preparation ?
_exptl_crystal_recrystallization_method
'The material was recrystallised from DCM by slow evaporation'
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.08
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0443
_diffrn_reflns_av_unetI/netI 0.0247
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 35
_diffrn_reflns_limit_h_min -35
_diffrn_reflns_limit_k_max 35
_diffrn_reflns_limit_k_min -35
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 93276
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 31.508
_diffrn_reflns_theta_min 1.654
_diffrn_ambient_temperature 100(2)
_diffrn_detector 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'Kappa diffractometer'
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'standard sealed X-ray tube'
_diffrn_source_type 'Siemens, KFF Mo 2K -90 C'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4493
_reflns_number_total 5684
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT V8.35A (Bruker, 2016)'
_computing_data_collection 'APEX 3 (Bruker, 2016) '
_computing_data_reduction 'SAINT V8.35A (Bruker, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XT (Sheldrick, 2015)'
_refine_diff_density_max 0.453
_refine_diff_density_min -0.395
_refine_diff_density_rms 0.057
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.046
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 239
_refine_ls_number_reflns 5684
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0528
_refine_ls_R_factor_gt 0.0341
_refine_ls_restrained_S_all 1.046
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+11.6815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0710
_refine_ls_wR_factor_ref 0.0778
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.48132(6) 0.22434(6) 0.46428(8) 0.0187(2) Uani 1 1 d . . . . .
H1 H 0.4365 0.2086 0.4602 0.022 Uiso 1 1 calc R . . . .
C2 C 0.51670(6) 0.20668(6) 0.41257(9) 0.0206(2) Uani 1 1 d . . . . .
H2 H 0.5013 0.1765 0.3659 0.025 Uiso 1 1 calc R . . . .
C3 C 0.58062(6) 0.24239(6) 0.44281(8) 0.0186(2) Uani 1 1 d . . . . .
H3 H 0.6155 0.2396 0.4185 0.022 Uiso 1 1 calc R . . . .
C5 C 0.63858(6) 0.40245(6) 0.72903(8) 0.0176(2) Uani 1 1 d . . . . .
H5 H 0.6818 0.4221 0.7486 0.021 Uiso 1 1 calc R . . . .
C6 C 0.59105(6) 0.41264(6) 0.76763(8) 0.0186(2) Uani 1 1 d . . . . .
H6 H 0.5963 0.4394 0.8164 0.022 Uiso 1 1 calc R . . . .
C7 C 0.53569(6) 0.37617(6) 0.72071(8) 0.0174(2) Uani 1 1 d . . . . .
H7 H 0.4952 0.3729 0.7308 0.021 Uiso 1 1 calc R . . . .
C8 C 0.50923(6) 0.30175(6) 0.59058(8) 0.0146(2) Uani 1 1 d . . . . .
C9 C 0.52448(6) 0.27076(6) 0.52519(8) 0.0152(2) Uani 1 1 d . . . . .
C10 C 0.55066(6) 0.34416(6) 0.65392(8) 0.0149(2) Uani 1 1 d . . . . .
C11 C 0.44162(6) 0.28867(6) 0.59248(8) 0.0158(2) Uani 1 1 d . . . . .
C12 C 0.39978(6) 0.25571(6) 0.66056(8) 0.0168(2) Uani 1 1 d . . . . .
C13 C 0.33697(6) 0.24303(6) 0.66232(9) 0.0198(2) Uani 1 1 d . . . . .
C14 C 0.31263(6) 0.26344(7) 0.59460(9) 0.0234(3) Uani 1 1 d . . . . .
C15 C 0.35448(7) 0.29688(7) 0.52647(9) 0.0233(3) Uani 1 1 d . . . . .
C16 C 0.41689(6) 0.30920(6) 0.52548(8) 0.0197(2) Uani 1 1 d . . . . .
C17 C 0.22145(7) 0.26029(8) 0.66510(10) 0.0292(3) Uani 1 1 d . . . . .
H17A H 0.2525 0.2768 0.7142 0.035 Uiso 1 1 calc R . . . .
H17B H 0.1840 0.2192 0.6835 0.035 Uiso 1 1 calc R . . . .
C18 C 0.20037(7) 0.30794(7) 0.64234(10) 0.0258(3) Uani 1 1 d . . . . .
H18A H 0.1717 0.2926 0.5906 0.031 Uiso 1 1 calc R . . . .
H18B H 0.2383 0.3497 0.6273 0.031 Uiso 1 1 calc R . . . .
C19 C 0.16513(7) 0.31630(7) 0.71981(9) 0.0257(3) Uani 1 1 d . . . . .
H19A H 0.1301 0.2736 0.7382 0.031 Uiso 1 1 calc R . . . .
H19B H 0.1953 0.3349 0.7696 0.031 Uiso 1 1 calc R . . . .
C20 C 0.13702(10) 0.35900(9) 0.69941(12) 0.0416(4) Uani 1 1 d . . . . .
H20A H 0.1075 0.3412 0.6497 0.062 Uiso 1 1 calc GR . . . .
H20B H 0.1717 0.4022 0.6846 0.062 Uiso 1 1 calc GR . . . .
H20C H 0.1138 0.3612 0.7508 0.062 Uiso 1 1 calc GR . . . .
F1 F 0.41894(4) 0.23223(4) 0.72653(5) 0.02119(16) Uani 1 1 d . . . . .
F2 F 0.29909(4) 0.20877(4) 0.72927(6) 0.02682(18) Uani 1 1 d . . . . .
F3 F 0.33339(5) 0.31816(5) 0.45967(6) 0.0354(2) Uani 1 1 d . . . . .
F4 F 0.45478(4) 0.34359(4) 0.45824(5) 0.02738(18) Uani 1 1 d . . . . .
Ga1 Ga 0.6667 0.3333 0.58435(2) 0.01305(6) Uani 1 3 d S T P . .
N1 N 0.58600(5) 0.28068(5) 0.50991(7) 0.0154(2) Uani 1 1 d . . . . .
N2 N 0.61515(5) 0.36156(5) 0.66134(7) 0.01504(19) Uani 1 1 d . . . . .
O1 O 0.25130(5) 0.25026(7) 0.58802(7) 0.0374(3) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0176(5) 0.0183(6) 0.0182(6) -0.0029(5) -0.0039(5) 0.0074(5)
C2 0.0234(6) 0.0195(6) 0.0177(6) -0.0070(5) -0.0044(5) 0.0098(5)
C3 0.0202(6) 0.0194(6) 0.0165(6) -0.0034(4) -0.0002(5) 0.0102(5)
C5 0.0201(6) 0.0172(5) 0.0153(5) -0.0030(4) -0.0023(4) 0.0092(5)
C6 0.0241(6) 0.0182(5) 0.0155(5) -0.0032(4) -0.0005(5) 0.0120(5)
C7 0.0206(6) 0.0178(5) 0.0169(6) -0.0002(4) 0.0013(5) 0.0119(5)
C8 0.0154(5) 0.0148(5) 0.0145(5) 0.0021(4) -0.0002(4) 0.0082(4)
C9 0.0157(5) 0.0146(5) 0.0148(5) -0.0006(4) -0.0013(4) 0.0070(4)
C10 0.0166(5) 0.0152(5) 0.0141(5) -0.0001(4) 0.0002(4) 0.0088(4)
C11 0.0161(5) 0.0168(5) 0.0165(5) -0.0022(4) -0.0020(4) 0.0097(4)
C12 0.0173(5) 0.0189(5) 0.0152(5) -0.0023(4) -0.0028(4) 0.0098(5)
C13 0.0168(5) 0.0213(6) 0.0195(6) -0.0052(5) 0.0005(5) 0.0080(5)
C14 0.0184(6) 0.0317(7) 0.0249(7) -0.0126(5) -0.0070(5) 0.0161(5)
C15 0.0299(7) 0.0308(7) 0.0199(6) -0.0056(5) -0.0088(5) 0.0233(6)
C16 0.0246(6) 0.0217(6) 0.0170(6) -0.0002(5) -0.0009(5) 0.0148(5)
C17 0.0217(6) 0.0492(9) 0.0242(7) -0.0126(6) -0.0052(5) 0.0233(7)
C18 0.0208(6) 0.0254(7) 0.0272(7) -0.0042(5) 0.0042(5) 0.0084(5)
C19 0.0234(6) 0.0315(7) 0.0237(7) -0.0023(5) 0.0026(5) 0.0150(6)
C20 0.0590(11) 0.0425(9) 0.0388(9) 0.0092(8) 0.0173(8) 0.0369(9)
F1 0.0218(4) 0.0243(4) 0.0167(4) 0.0034(3) -0.0016(3) 0.0111(3)
F2 0.0191(4) 0.0298(4) 0.0257(4) -0.0026(3) 0.0055(3) 0.0079(3)
F3 0.0451(5) 0.0540(6) 0.0276(5) -0.0022(4) -0.0114(4) 0.0401(5)
F4 0.0339(5) 0.0320(4) 0.0207(4) 0.0088(3) 0.0033(3) 0.0198(4)
Ga1 0.01376(7) 0.01376(7) 0.01164(10) 0.000 0.000 0.00688(3)
N1 0.0166(5) 0.0161(5) 0.0135(5) -0.0015(4) 0.0001(4) 0.0083(4)
N2 0.0155(5) 0.0160(5) 0.0137(5) -0.0016(4) -0.0011(4) 0.0079(4)
O1 0.0234(5) 0.0702(8) 0.0288(6) -0.0248(6) -0.0117(4) 0.0311(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9500 . ?
C1 C2 1.3755(18) . ?
C1 C9 1.4254(16) . ?
C2 H2 0.9500 . ?
C2 C3 1.4139(18) . ?
C3 H3 0.9500 . ?
C3 N1 1.3400(16) . ?
C5 H5 0.9500 . ?
C5 C6 1.4138(17) . ?
C5 N2 1.3413(15) . ?
C6 H6 0.9500 . ?
C6 C7 1.3749(18) . ?
C7 H7 0.9500 . ?
C7 C10 1.4283(16) . ?
C8 C9 1.4006(17) . ?
C8 C10 1.3978(17) . ?
C8 C11 1.4964(16) . ?
C9 N1 1.3976(15) . ?
C10 N2 1.3967(15) . ?
C11 C12 1.3872(17) . ?
C11 C16 1.3921(17) . ?
C12 C13 1.3861(17) . ?
C12 F1 1.3439(14) . ?
C13 C14 1.3932(19) . ?
C13 F2 1.3429(15) . ?
C14 C15 1.390(2) . ?
C14 O1 1.3507(16) . ?
C15 C16 1.3793(19) . ?
C15 F3 1.3490(15) . ?
C16 F4 1.3472(15) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.509(2) . ?
C17 O1 1.4598(17) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.5259(19) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.520(2) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
Ga1 N1 2.0516(10) 2_655 ?
Ga1 N1 2.0516(10) . ?
Ga1 N1 2.0516(10) 3_665 ?
Ga1 N2 2.0553(10) 2_655 ?
Ga1 N2 2.0553(10) . ?
Ga1 N2 2.0553(10) 3_665 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 126.4 . . ?
C2 C1 C9 107.14(11) . . ?
C9 C1 H1 126.4 . . ?
C1 C2 H2 126.9 . . ?
C1 C2 C3 106.23(11) . . ?
C3 C2 H2 126.9 . . ?
C2 C3 H3 124.2 . . ?
N1 C3 C2 111.65(11) . . ?
N1 C3 H3 124.2 . . ?
C6 C5 H5 124.2 . . ?
N2 C5 H5 124.2 . . ?
N2 C5 C6 111.60(11) . . ?
C5 C6 H6 126.8 . . ?
C7 C6 C5 106.45(11) . . ?
C7 C6 H6 126.8 . . ?
C6 C7 H7 126.6 . . ?
C6 C7 C10 106.87(11) . . ?
C10 C7 H7 126.6 . . ?
C9 C8 C11 116.72(10) . . ?
C10 C8 C9 126.87(11) . . ?
C10 C8 C11 116.41(10) . . ?
C8 C9 C1 126.83(11) . . ?
N1 C9 C1 108.70(10) . . ?
N1 C9 C8 124.47(11) . . ?
C8 C10 C7 127.36(11) . . ?
N2 C10 C7 108.87(10) . . ?
N2 C10 C8 123.77(11) . . ?
C12 C11 C8 122.52(11) . . ?
C12 C11 C16 115.82(11) . . ?
C16 C11 C8 121.66(11) . . ?
C13 C12 C11 122.76(12) . . ?
F1 C12 C11 119.83(11) . . ?
F1 C12 C13 117.35(11) . . ?
C12 C13 C14 120.91(12) . . ?
F2 C13 C12 118.79(12) . . ?
F2 C13 C14 120.27(12) . . ?
C15 C14 C13 116.57(12) . . ?
O1 C14 C13 125.18(14) . . ?
O1 C14 C15 118.15(13) . . ?
C16 C15 C14 121.98(12) . . ?
F3 C15 C14 118.88(12) . . ?
F3 C15 C16 119.15(13) . . ?
C15 C16 C11 121.97(12) . . ?
F4 C16 C11 119.91(11) . . ?
F4 C16 C15 118.10(11) . . ?
H17A C17 H17B 108.3 . . ?
C18 C17 H17A 109.9 . . ?
C18 C17 H17B 109.9 . . ?
O1 C17 H17A 109.9 . . ?
O1 C17 H17B 109.9 . . ?
O1 C17 C18 108.75(13) . . ?
C17 C18 H18A 109.6 . . ?
C17 C18 H18B 109.6 . . ?
C17 C18 C19 110.07(12) . . ?
H18A C18 H18B 108.2 . . ?
C19 C18 H18A 109.6 . . ?
C19 C18 H18B 109.6 . . ?
C18 C19 H19A 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 C18 113.34(13) . . ?
C20 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 Ga1 N1 92.32(4) 2_655 . ?
N1 Ga1 N1 92.32(4) . 3_665 ?
N1 Ga1 N1 92.32(4) 2_655 3_665 ?
N1 Ga1 N2 88.79(4) 3_665 3_665 ?
N1 Ga1 N2 88.28(4) 2_655 3_665 ?
N1 Ga1 N2 88.79(4) . . ?
N1 Ga1 N2 88.79(4) 2_655 2_655 ?
N1 Ga1 N2 88.28(4) . 2_655 ?
N1 Ga1 N2 178.71(4) . 3_665 ?
N1 Ga1 N2 88.28(4) 3_665 . ?
N1 Ga1 N2 178.71(4) 3_665 2_655 ?
N1 Ga1 N2 178.71(4) 2_655 . ?
N2 Ga1 N2 90.60(4) 2_655 . ?
N2 Ga1 N2 90.60(4) 2_655 3_665 ?
N2 Ga1 N2 90.60(4) 3_665 . ?
C3 N1 C9 106.28(10) . . ?
C3 N1 Ga1 125.73(8) . . ?
C9 N1 Ga1 127.51(8) . . ?
C5 N2 C10 106.21(10) . . ?
C5 N2 Ga1 125.50(8) . . ?
C10 N2 Ga1 128.27(8) . . ?
C14 O1 C17 118.20(11) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C3 H3 N1 0.95 2.60 3.0729(16) 111.3 2_655
C5 H5 N2 0.95 2.53 3.0154(16) 111.8 3_665
C6 H6 F1 0.95 2.41 3.3053(14) 157.8 17_556
C17 H17A F3 0.99 2.41 3.3445(18) 158.2 5
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 N1 0.01(15) . . . . ?
C1 C9 N1 C3 0.22(14) . . . . ?
C1 C9 N1 Ga1 -172.16(8) . . . . ?
C2 C1 C9 C8 -179.78(12) . . . . ?
C2 C1 C9 N1 -0.22(14) . . . . ?
C2 C3 N1 C9 -0.14(14) . . . . ?
C2 C3 N1 Ga1 172.42(9) . . . . ?
C5 C6 C7 C10 0.03(14) . . . . ?
C6 C5 N2 C10 0.34(14) . . . . ?
C6 C5 N2 Ga1 179.12(8) . . . . ?
C6 C7 C10 C8 179.77(12) . . . . ?
C6 C7 C10 N2 0.17(14) . . . . ?
C7 C10 N2 C5 -0.31(13) . . . . ?
C7 C10 N2 Ga1 -179.05(8) . . . . ?
C8 C9 N1 C3 179.79(12) . . . . ?
C8 C9 N1 Ga1 7.41(17) . . . . ?
C8 C10 N2 C5 -179.93(11) . . . . ?
C8 C10 N2 Ga1 1.33(17) . . . . ?
C8 C11 C12 C13 -179.49(12) . . . . ?
C8 C11 C12 F1 -2.39(18) . . . . ?
C8 C11 C16 C15 179.48(12) . . . . ?
C8 C11 C16 F4 -2.25(18) . . . . ?
C9 C1 C2 C3 0.13(14) . . . . ?
C9 C8 C10 C7 179.81(12) . . . . ?
C9 C8 C10 N2 -0.6(2) . . . . ?
C9 C8 C11 C12 113.09(13) . . . . ?
C9 C8 C11 C16 -67.05(16) . . . . ?
C10 C8 C9 C1 175.57(12) . . . . ?
C10 C8 C9 N1 -3.9(2) . . . . ?
C10 C8 C11 C12 -67.48(16) . . . . ?
C10 C8 C11 C16 112.39(13) . . . . ?
C11 C8 C9 C1 -5.07(18) . . . . ?
C11 C8 C9 N1 175.44(11) . . . . ?
C11 C8 C10 C7 0.44(18) . . . . ?
C11 C8 C10 N2 179.99(11) . . . . ?
C11 C12 C13 C14 -0.2(2) . . . . ?
C11 C12 C13 F2 177.60(11) . . . . ?
C12 C11 C16 C15 -0.65(18) . . . . ?
C12 C11 C16 F4 177.62(11) . . . . ?
C12 C13 C14 C15 -0.19(19) . . . . ?
C12 C13 C14 O1 176.00(13) . . . . ?
C13 C14 C15 C16 0.2(2) . . . . ?
C13 C14 C15 F3 -179.44(12) . . . . ?
C13 C14 O1 C17 48.0(2) . . . . ?
C14 C15 C16 C11 0.3(2) . . . . ?
C14 C15 C16 F4 -178.04(12) . . . . ?
C15 C14 O1 C17 -135.86(15) . . . . ?
C16 C11 C12 C13 0.64(18) . . . . ?
C16 C11 C12 F1 177.74(11) . . . . ?
C17 C18 C19 C20 -174.79(14) . . . . ?
C18 C17 O1 C14 121.08(14) . . . . ?
F1 C12 C13 C14 -177.40(11) . . . . ?
F1 C12 C13 F2 0.44(17) . . . . ?
F2 C13 C14 C15 -178.00(12) . . . . ?
F2 C13 C14 O1 -1.8(2) . . . . ?
F3 C15 C16 C11 179.87(12) . . . . ?
F3 C15 C16 F4 1.57(19) . . . . ?
N2 C5 C6 C7 -0.24(15) . . . . ?
O1 C14 C15 C16 -176.29(13) . . . . ?
O1 C14 C15 F3 4.09(19) . . . . ?
O1 C17 C18 C19 176.41(11) . . . . ?
_shelx_res_file
;
kjf141.res created by SHELXL-2014/7
TITL kjf141_a.res in R-3
REM Old TITL kjf141 in R-3
REM SHELXT solution in R-3
REM R1 0.094, Rweak 0.006, Alpha 0.020, Orientation as input
REM Formula found by SHELXT: C57 N9 F12 Ga
CELL 0.71073 24.0883 24.0883 15.2527 90 90 120
ZERR 6 0.001 0.001 0.0007 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H F Ga N O
UNIT 342 270 72 6 36 18
EQIV $1 1-Y,+X-Y,+Z
EQIV $2 0.333+Y,0.667-X+Y,1.667-Z
EQIV $3 1+Y-X,1-X,+Z
EQIV $4 0.667-Y,0.333+X-Y,0.333+Z
L.S. 10
PLAN 20
SIZE 0.08 0.08 0.5
TEMP -173(2)
HTAB C3 N1_$1
HTAB C6 F1_$2
HTAB C5 N2_$3
HTAB C17 F3_$4
BOND $H
HTAB
WPDB
MORE -1
CONF
fmap 2
acta 52
REM
REM
REM
WGHT 0.030000 11.681500
FVAR 0.15179
C1 1 0.481322 0.224343 0.464278 11.00000 0.01756 0.01826 =
0.01817 -0.00295 -0.00388 0.00739
AFIX 43
H1 2 0.436530 0.208568 0.460169 11.00000 -1.20000
AFIX 0
C2 1 0.516700 0.206679 0.412570 11.00000 0.02338 0.01948 =
0.01768 -0.00696 -0.00438 0.00979
AFIX 43
H2 2 0.501276 0.176531 0.365893 11.00000 -1.20000
AFIX 0
C3 1 0.580624 0.242386 0.442809 11.00000 0.02019 0.01940 =
0.01654 -0.00342 -0.00016 0.01019
AFIX 43
H3 2 0.615461 0.239575 0.418549 11.00000 -1.20000
AFIX 0
C5 1 0.638584 0.402450 0.729031 11.00000 0.02006 0.01721 =
0.01528 -0.00304 -0.00230 0.00916
AFIX 43
H5 2 0.681758 0.422125 0.748610 11.00000 -1.20000
AFIX 0
C6 1 0.591051 0.412639 0.767627 11.00000 0.02411 0.01822 =
0.01549 -0.00324 -0.00052 0.01204
AFIX 43
H6 2 0.596320 0.439404 0.816361 11.00000 -1.20000
AFIX 0
C7 1 0.535694 0.376166 0.720713 11.00000 0.02056 0.01777 =
0.01688 -0.00023 0.00133 0.01185
AFIX 43
H7 2 0.495238 0.372881 0.730793 11.00000 -1.20000
AFIX 0
C8 1 0.509226 0.301752 0.590576 11.00000 0.01545 0.01476 =
0.01452 0.00207 -0.00016 0.00817
C9 1 0.524484 0.270759 0.525186 11.00000 0.01568 0.01458 =
0.01475 -0.00063 -0.00125 0.00704
C10 1 0.550663 0.344164 0.653920 11.00000 0.01656 0.01520 =
0.01412 -0.00012 0.00017 0.00879
C11 1 0.441619 0.288672 0.592477 11.00000 0.01610 0.01678 =
0.01652 -0.00218 -0.00198 0.00975
C12 1 0.399785 0.255705 0.660560 11.00000 0.01726 0.01891 =
0.01517 -0.00227 -0.00281 0.00983
C13 1 0.336972 0.243030 0.662322 11.00000 0.01679 0.02127 =
0.01948 -0.00522 0.00050 0.00800
C14 1 0.312625 0.263441 0.594595 11.00000 0.01839 0.03172 =
0.02489 -0.01262 -0.00701 0.01609
C15 1 0.354481 0.296876 0.526470 11.00000 0.02992 0.03078 =
0.01994 -0.00556 -0.00877 0.02326
C16 1 0.416894 0.309197 0.525481 11.00000 0.02462 0.02170 =
0.01697 -0.00023 -0.00090 0.01475
C17 1 0.221451 0.260293 0.665099 11.00000 0.02170 0.04915 =
0.02418 -0.01264 -0.00521 0.02329
AFIX 23
H17A 2 0.252460 0.276831 0.714207 11.00000 -1.20000
H17B 2 0.184000 0.219185 0.683529 11.00000 -1.20000
AFIX 0
C18 1 0.200367 0.307937 0.642343 11.00000 0.02078 0.02537 =
0.02721 -0.00415 0.00423 0.00841
AFIX 23
H18A 2 0.171711 0.292593 0.590630 11.00000 -1.20000
H18B 2 0.238271 0.349716 0.627321 11.00000 -1.20000
AFIX 0
C19 1 0.165127 0.316299 0.719814 11.00000 0.02342 0.03154 =
0.02369 -0.00233 0.00260 0.01496
AFIX 23
H19A 2 0.130098 0.273622 0.738211 11.00000 -1.20000
H19B 2 0.195270 0.334946 0.769627 11.00000 -1.20000
AFIX 0
C20 1 0.137017 0.359000 0.699407 11.00000 0.05895 0.04250 =
0.03876 0.00921 0.01733 0.03689
AFIX 137
H20A 2 0.107499 0.341180 0.649658 11.00000 -1.50000
H20B 2 0.171677 0.402151 0.684636 11.00000 -1.50000
H20C 2 0.113750 0.361204 0.750768 11.00000 -1.50000
AFIX 0
F1 3 0.418942 0.232231 0.726530 11.00000 0.02185 0.02435 =
0.01672 0.00336 -0.00157 0.01106
F2 3 0.299092 0.208768 0.729266 11.00000 0.01909 0.02983 =
0.02572 -0.00261 0.00547 0.00787
F3 3 0.333393 0.318162 0.459666 11.00000 0.04509 0.05401 =
0.02759 -0.00215 -0.01144 0.04012
F4 3 0.454783 0.343588 0.458241 11.00000 0.03388 0.03196 =
0.02073 0.00875 0.00331 0.01977
GA1 4 0.666667 0.333333 0.584353 10.33333 0.01376 0.01376 =
0.01164 0.00000 0.00000 0.00688
N1 5 0.586004 0.280680 0.509911 11.00000 0.01664 0.01614 =
0.01346 -0.00155 0.00005 0.00833
N2 5 0.615152 0.361556 0.661337 11.00000 0.01545 0.01601 =
0.01372 -0.00164 -0.00112 0.00791
O1 6 0.251296 0.250265 0.588017 11.00000 0.02336 0.07016 =
0.02884 -0.02477 -0.01169 0.03107
HKLF 4
REM kjf141_a.res in R-3
REM R1 = 0.0341 for 4493 Fo > 4sig(Fo) and 0.0528 for all 5684 data
REM 239 parameters refined using 0 restraints
END
WGHT 0.0300 11.6731
REM Instructions for potential hydrogen bonds
HTAB C3 N1_$1
HTAB C5 N2_$3
HTAB C6 F1_$2
HTAB C17 F3_$4
REM Highest difference peak 0.453, deepest hole -0.395, 1-sigma level 0.057
Q1 1 0.5413 0.3593 0.6835 11.00000 0.05 0.45
Q2 1 0.5209 0.2921 0.5579 11.00000 0.05 0.41
Q3 1 0.5003 0.2445 0.5006 11.00000 0.05 0.41
Q4 1 0.5505 0.2235 0.4267 11.00000 0.05 0.40
Q5 1 0.5636 0.3914 0.7480 11.00000 0.05 0.39
Q6 1 0.5271 0.3151 0.6346 11.00000 0.05 0.39
Q7 1 0.3666 0.2434 0.6552 11.00000 0.05 0.39
Q8 1 0.6108 0.4075 0.7470 11.00000 0.05 0.39
Q9 1 0.3813 0.2910 0.5216 11.00000 0.05 0.39
Q10 1 0.5851 0.2644 0.4734 11.00000 0.05 0.38
Q11 1 0.4735 0.2967 0.5923 11.00000 0.05 0.36
Q12 1 0.6268 0.3809 0.6935 11.00000 0.05 0.36
Q13 1 0.4185 0.2689 0.6241 11.00000 0.05 0.34
Q14 1 0.3325 0.2696 0.5512 11.00000 0.05 0.34
Q15 1 0.2124 0.2897 0.6604 11.00000 0.05 0.33
Q16 1 0.4965 0.2183 0.4300 11.00000 0.05 0.33
Q17 1 0.3219 0.2623 0.6370 11.00000 0.05 0.32
Q18 1 0.4210 0.2917 0.5571 11.00000 0.05 0.31
Q19 1 0.5539 0.2777 0.5219 11.00000 0.05 0.29
Q20 1 0.3193 0.2383 0.6193 11.00000 0.05 0.28
;
_shelx_res_checksum 76037
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN micromount using oil'
_olex2_submission_special_instructions 'No special instructions were received'