#==============================================================================
data_global
loop_
_journal_name_full 'European Journal of Chemistry'
_journal_coden_ASTM EJCUA9
_journal_volume 12
_journal_issue 3
_journal_year 2021
_journal_page_first 323
_journal_page_last 328
#==============================================================================
_publ_contact_author
;
Muhammad Nawaz Tahir
University of Sargodha
Department of Physics
Sargodha
Pakistan
;
_publ_contact_author_phone '0092 48 92 30 914'
_publ_contact_author_fax '0092 48 32 22 121'
_publ_contact_author_email 'dmntahir_uos@yahoo.com'
#==============================================================
loop_
_publ_author_name
_publ_author_address
'Syed Muddassir Ali Mashhadi'
;
Department of Chemistry
Allama Iqbal Open University
Sector H-8/4
Islamabad
Pakistan
;
'Uzma Yunus'
;
Department of Chemistry
Allama Iqbal Open University
Sector H-8/4
Islamabad
Pakistan
;
'Muhammad Nawaz Tahir'
;
Department of Physics
University of Sargodha
Sargodha
Pakistan
;
_audit_creation_date ?
_audit_creation_method ?
_publ_section_references
;
Bruker (2005). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2007). APEX2 and SAINT. Bruker AXS Inc.,
Madison, Wisconsin, USA.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
Sheldrick, G. M. (2015). Acta Cryst. C71, 3--8.
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
;
data_L26AIOU
_audit_creation_method 'SHELXL-2014/7'
_shelx_SHELXL_version_number '2014/7'
_chemical_name_common ?
_chemical_absolute_configuration '.'
_chemical_name_systematic
;
4-(6-Carboxy-9-fluoro-3-methyl-7-oxo-2,3-dihydro-7H-[1,4]oxazino[2,3,4-ij]
quinolin-10-yl)-1-methylpiperazin-1-ium 2,6-dihydroxybenzoate
;
_chemical_formula_moiety 'C25 H26 F N3 O8'
_chemical_formula_sum 'C25 H26 F N3 O8'
_chemical_formula_iupac 'C25 H26 F N3 O8'
_chemical_formula_weight 515.49
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'
'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'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 7.0037(8)
_cell_length_b 12.764(3)
_cell_length_c 13.909(3)
_cell_angle_alpha 104.821(4)
_cell_angle_beta 92.039(4)
_cell_angle_gamma 95.334(4)
_cell_volume 1194.6(4)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 2383
_cell_measurement_theta_min 2.524
_cell_measurement_theta_max 27.093
_cell_measurement_temperature 296(2)
_exptl_crystal_description needle
_exptl_crystal_colour 'white'
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.18
_exptl_crystal_density_diffrn 1.433
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 540
_exptl_absorpt_coefficient_mu 0.113
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Bruker, 2005)'
_shelx_estimated_absorpt_T_min 0.956
_shelx_estimated_absorpt_T_max 0.980
_exptl_absorpt_correction_T_min 0.9503
_exptl_absorpt_correction_T_max 0.9856
_exptl_special_details
;
;
_diffrn_ambient_temperature 296(2)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Kappa APEXII CCD'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean 0.78
_diffrn_reflns_number 16879
_diffrn_reflns_av_unetI/netI 0.0975
_diffrn_reflns_av_R_equivalents 0.0663
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 2.524
_diffrn_reflns_theta_max 27.093
_diffrn_reflns_theta_full 27.090
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.978
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F^2^, conventional
R-factors R are based on F, with F set to zero for
negative F^2^. The threshold expression of F^2^ >
\s(F^2^) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F^2^ are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger.
;
_reflns_number_total 5139
_reflns_number_gt 2383
_reflns_threshold_expression I>2\s(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.2040
_refine_ls_R_factor_gt 0.1121
_refine_ls_wR_factor_ref 0.2505
_refine_ls_wR_factor_gt 0.2189
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_restrained_S_all 1.049
_refine_ls_number_reflns 5183
_refine_ls_number_parameters 303
_refine_ls_number_restraints 14
_refine_ls_hydrogen_treatment mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+5.3089P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef 0.0048(11)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'SAINT (Bruker, 2007)'
_computing_data_reduction 'SAINT (Bruker, 2007)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009)'
_computing_publication_material
;
WinGX (Farrugia, 1999) and PLATON (Spek, 2009)
;
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
F1 F 0.7389(6) -0.0768(3) 0.2853(3) 0.0724(12) Uani 1 1 d . . . . .
O1 O 0.7058(7) -0.1765(4) -0.2691(3) 0.0651(13) Uani 1 1 d . . . . .
H1 H 0.7242 -0.1993 -0.2199 0.098 Uiso 1 1 calc R U . . .
O2 O 0.7207(7) -0.0166(4) -0.3030(3) 0.0697(14) Uani 1 1 d . . . . .
O3 O 0.7078(6) -0.1873(3) -0.0886(3) 0.0553(11) Uani 1 1 d . . . . .
O4 O 0.8477(7) 0.2571(3) 0.1988(3) 0.0615(13) Uani 1 1 d D . . . .
N1 N 0.7813(8) 0.1475(4) -0.0034(3) 0.0516(14) Uani 1 1 d D . . . .
N2 N 0.7948(8) 0.1470(4) 0.3463(3) 0.0565(15) Uani 1 1 d . . . . .
N3 N 0.7144(7) 0.2152(4) 0.5493(3) 0.0464(13) Uani 1 1 d . . . . .
H3 H 0.801(9) 0.275(5) 0.580(4) 0.056 Uiso 1 1 d . U . . .
C1 C 0.7214(8) -0.0681(5) -0.2420(5) 0.0486(16) Uani 1 1 d . . . . .
C2 C 0.7390(8) -0.0191(5) -0.1326(4) 0.0392(13) Uani 1 1 d . . . . .
C3 C 0.7307(7) -0.0838(5) -0.0621(4) 0.0401(14) Uani 1 1 d . . . . .
C4 C 0.7475(7) -0.0245(5) 0.0416(4) 0.0380(13) Uani 1 1 d . . . . .
C5 C 0.7759(8) 0.0899(4) 0.0701(4) 0.0371(13) Uani 1 1 d . . . . .
C6 C 0.7616(8) 0.0907(5) -0.0993(4) 0.0479(15) Uani 1 1 d . . . . .
H6 H 0.7636 0.1302 -0.1469 0.058 Uiso 1 1 calc R U . . .
C7 C 0.7416(8) -0.0804(5) 0.1173(4) 0.0426(14) Uani 1 1 d . . . . .
H7 H 0.7259 -0.1562 0.1010 0.051 Uiso 1 1 calc R U . . .
C8 C 0.7588(8) -0.0229(5) 0.2127(4) 0.0463(15) Uani 1 1 d . . . . .
C9 C 0.7873(8) 0.0917(5) 0.2458(4) 0.0436(14) Uani 1 1 d . . . . .
C10 C 0.8025(8) 0.1465(4) 0.1707(4) 0.0434(14) Uani 1 1 d . . . . .
C11A C 0.791(3) 0.3118(12) 0.1322(8) 0.061(3) Uani 0.541(12) 1 d D . P A 1
H11A H 0.8450 0.3873 0.1554 0.073 Uiso 0.541(12) 1 calc R U P A 1
H11B H 0.6519 0.3108 0.1313 0.073 Uiso 0.541(12) 1 calc R U P A 1
C12A C 0.846(2) 0.2673(9) 0.0271(8) 0.061(3) Uani 0.541(12) 1 d D . P A 1
H12A H 0.9864 0.2787 0.0248 0.073 Uiso 0.541(12) 1 calc R U P A 1
C13A C 0.752(3) 0.3298(13) -0.0370(11) 0.061(3) Uani 0.541(12) 1 d D . P A 1
H13A H 0.6182 0.3042 -0.0491 0.091 Uiso 0.541(12) 1 calc R U P A 1
H13B H 0.8123 0.3188 -0.0994 0.091 Uiso 0.541(12) 1 calc R U P A 1
H13C H 0.7670 0.4060 -0.0034 0.091 Uiso 0.541(12) 1 calc R U P A 1
C11B C 0.877(3) 0.3058(14) 0.1197(10) 0.061(3) Uani 0.459(12) 1 d D . P A 2
H11C H 1.0082 0.2983 0.1011 0.073 Uiso 0.459(12) 1 calc R U P A 2
H11D H 0.8664 0.3831 0.1449 0.073 Uiso 0.459(12) 1 calc R U P A 2
C12B C 0.749(3) 0.2652(10) 0.0277(10) 0.061(3) Uani 0.459(12) 1 d D . P A 2
H12B H 0.6143 0.2754 0.0401 0.073 Uiso 0.459(12) 1 calc R U P A 2
C13B C 0.822(3) 0.3188(16) -0.0514(13) 0.061(3) Uani 0.459(12) 1 d D . P A 2
H13D H 0.8168 0.3961 -0.0289 0.091 Uiso 0.459(12) 1 calc R U P A 2
H13E H 0.7427 0.2903 -0.1119 0.091 Uiso 0.459(12) 1 calc R U P A 2
H13F H 0.9520 0.3041 -0.0634 0.091 Uiso 0.459(12) 1 calc R U P A 2
C14 C 0.9108(9) 0.1156(6) 0.4215(4) 0.0574(18) Uani 1 1 d . . . . .
H14A H 1.0221 0.1687 0.4440 0.069 Uiso 1 1 calc R U . . .
H14B H 0.9556 0.0453 0.3931 0.069 Uiso 1 1 calc R U . . .
C15 C 0.7914(11) 0.1098(6) 0.5080(5) 0.066(2) Uani 1 1 d . . . . .
H15A H 0.6859 0.0526 0.4862 0.080 Uiso 1 1 calc R U . . .
H15B H 0.8695 0.0919 0.5594 0.080 Uiso 1 1 calc R U . . .
C16 C 0.6069(9) 0.2510(5) 0.4712(4) 0.0493(15) Uani 1 1 d . . . . .
H16A H 0.5697 0.3233 0.4993 0.059 Uiso 1 1 calc R U . . .
H16B H 0.4908 0.2017 0.4485 0.059 Uiso 1 1 calc R U . . .
C17 C 0.7276(9) 0.2525(5) 0.3846(4) 0.0512(16) Uani 1 1 d . . . . .
H17A H 0.6522 0.2709 0.3325 0.061 Uiso 1 1 calc R U . . .
H17B H 0.8365 0.3075 0.4055 0.061 Uiso 1 1 calc R U . . .
C18 C 0.5956(11) 0.2128(6) 0.6354(5) 0.077(2) Uani 1 1 d . . . . .
H18A H 0.4668 0.1826 0.6115 0.115 Uiso 1 1 calc R U . . .
H18B H 0.5941 0.2856 0.6766 0.115 Uiso 1 1 calc R U . . .
H18C H 0.6493 0.1686 0.6737 0.115 Uiso 1 1 calc R U . . .
O5 O 0.9765(7) 0.6449(5) 0.3948(4) 0.0863(17) Uani 1 1 d . . . . .
O6 O 0.9710(9) 0.6916(6) 0.2522(5) 0.109(2) Uani 1 1 d . . . . .
C19 C 0.8978(11) 0.6394(7) 0.3085(6) 0.079(2) Uani 1 1 d D . . . .
O7A O 0.6957(17) 0.5877(10) 0.1156(8) 0.0762(10) Uani 0.541(12) 1 d D . P A 1
H7A H 0.8102 0.6049 0.1320 0.114 Uiso 0.541(12) 1 calc R U P A 1
O8A O 0.712(2) 0.5115(9) 0.4350(9) 0.0762(10) Uani 0.541(12) 1 d D . P A 1
H8A H 0.7968 0.5620 0.4564 0.114 Uiso 0.541(12) 1 calc R U P A 1
C20A C 0.7091(19) 0.5666(16) 0.2794(13) 0.0762(10) Uani 0.541(12) 1 d DG . P A 1
C21A C 0.608(2) 0.5530(14) 0.1885(10) 0.0762(10) Uani 0.541(12) 1 d DG . P A 1
C22A C 0.4257(19) 0.4956(11) 0.1707(7) 0.0762(10) Uani 0.541(12) 1 d G . P A 1
H22A H 0.3579 0.4865 0.1099 0.091 Uiso 0.541(12) 1 calc R U P A 1
C23A C 0.3452(14) 0.4519(11) 0.2437(9) 0.0762(10) Uani 0.541(12) 1 d G . P A 1
H23A H 0.2235 0.4135 0.2317 0.091 Uiso 0.541(12) 1 calc R U P A 1
C24A C 0.4467(19) 0.4655(12) 0.3345(8) 0.0762(10) Uani 0.541(12) 1 d G . P A 1
H24A H 0.3928 0.4362 0.3833 0.091 Uiso 0.541(12) 1 calc R U P A 1
C25A C 0.629(2) 0.5229(15) 0.3524(9) 0.0762(10) Uani 0.541(12) 1 d DG . P A 1
O7B O 0.702(2) 0.6365(12) 0.1310(10) 0.0762(10) Uani 0.459(12) 1 d D . P A 2
H7B H 0.8153 0.6306 0.1205 0.114 Uiso 0.459(12) 1 calc R U P A 2
O8B O 0.688(3) 0.5420(12) 0.4387(11) 0.0762(10) Uani 0.459(12) 1 d D . P A 2
H8B H 0.7477 0.6029 0.4544 0.114 Uiso 0.459(12) 1 calc R U P A 2
C20B C 0.714(3) 0.5755(19) 0.2810(15) 0.0762(10) Uani 0.459(12) 1 d DG . P A 2
C21B C 0.640(3) 0.5680(16) 0.1852(13) 0.0762(10) Uani 0.459(12) 1 d DG . P A 2
C22B C 0.468(2) 0.5039(14) 0.1490(9) 0.0762(10) Uani 0.459(12) 1 d G . P A 2
H22B H 0.4185 0.4989 0.0849 0.091 Uiso 0.459(12) 1 calc R U P A 2
C23B C 0.3708(18) 0.4472(12) 0.2087(10) 0.0762(10) Uani 0.459(12) 1 d G . P A 2
H23B H 0.2560 0.4043 0.1845 0.091 Uiso 0.459(12) 1 calc R U P A 2
C24B C 0.445(2) 0.4546(13) 0.3045(9) 0.0762(10) Uani 0.459(12) 1 d G . P A 2
H24B H 0.3799 0.4167 0.3444 0.091 Uiso 0.459(12) 1 calc R U P A 2
C25B C 0.617(3) 0.5188(18) 0.3407(10) 0.0762(10) Uani 0.459(12) 1 d DG . P A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
F1 0.104(3) 0.068(3) 0.061(2) 0.036(2) 0.031(2) 0.021(2)
O1 0.073(3) 0.062(3) 0.050(3) -0.004(2) -0.008(2) 0.014(3)
O2 0.088(4) 0.083(4) 0.041(3) 0.018(2) 0.004(2) 0.020(3)
O3 0.055(3) 0.042(3) 0.063(3) 0.004(2) 0.003(2) 0.002(2)
O4 0.097(4) 0.043(3) 0.041(2) 0.0068(19) 0.003(2) -0.002(2)
N1 0.078(4) 0.038(3) 0.039(3) 0.008(2) 0.003(3) 0.013(3)
N2 0.077(4) 0.064(4) 0.035(3) 0.013(2) 0.010(3) 0.035(3)
N3 0.052(3) 0.054(3) 0.038(3) 0.015(2) 0.014(2) 0.016(3)
C1 0.036(4) 0.056(4) 0.047(4) -0.003(3) 0.002(3) 0.014(3)
C2 0.029(3) 0.045(4) 0.042(3) 0.007(3) 0.001(2) 0.009(3)
C3 0.019(3) 0.046(4) 0.052(4) 0.006(3) 0.001(2) 0.005(2)
C4 0.025(3) 0.044(3) 0.046(3) 0.014(3) 0.009(2) 0.002(2)
C5 0.036(3) 0.044(3) 0.034(3) 0.014(3) 0.007(2) 0.005(3)
C6 0.052(4) 0.053(4) 0.040(3) 0.015(3) 0.004(3) 0.008(3)
C7 0.037(3) 0.041(3) 0.052(4) 0.010(3) 0.012(3) 0.011(3)
C8 0.041(4) 0.056(4) 0.050(4) 0.023(3) 0.020(3) 0.014(3)
C9 0.044(4) 0.047(4) 0.043(3) 0.013(3) 0.006(3) 0.013(3)
C10 0.051(4) 0.035(3) 0.043(3) 0.007(3) 0.007(3) 0.005(3)
C11A 0.092(8) 0.044(3) 0.048(3) 0.010(2) 0.013(4) 0.021(4)
C12A 0.092(8) 0.044(3) 0.048(3) 0.010(2) 0.013(4) 0.021(4)
C13A 0.092(8) 0.044(3) 0.048(3) 0.010(2) 0.013(4) 0.021(4)
C11B 0.092(8) 0.044(3) 0.048(3) 0.010(2) 0.013(4) 0.021(4)
C12B 0.092(8) 0.044(3) 0.048(3) 0.010(2) 0.013(4) 0.021(4)
C13B 0.092(8) 0.044(3) 0.048(3) 0.010(2) 0.013(4) 0.021(4)
C14 0.056(4) 0.085(5) 0.040(3) 0.021(3) 0.010(3) 0.038(4)
C15 0.087(5) 0.075(5) 0.051(4) 0.028(4) 0.025(4) 0.037(4)
C16 0.047(4) 0.052(4) 0.049(4) 0.008(3) 0.004(3) 0.015(3)
C17 0.065(4) 0.052(4) 0.040(3) 0.013(3) 0.003(3) 0.021(3)
C18 0.088(6) 0.086(6) 0.069(5) 0.031(4) 0.041(4) 0.029(5)
O5 0.069(4) 0.113(5) 0.064(3) 0.011(3) -0.017(3) -0.012(3)
O6 0.100(5) 0.140(6) 0.092(5) 0.041(4) 0.005(4) 0.002(4)
C19 0.085(6) 0.082(6) 0.064(5) 0.004(4) 0.000(5) 0.022(5)
O7A 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
O8A 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
C20A 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
C21A 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
C22A 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
C23A 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
C24A 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
C25A 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
O7B 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
O8B 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
C20B 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
C21B 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
C22B 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
C23B 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
C24B 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
C25B 0.093(2) 0.056(2) 0.073(2) 0.007(2) -0.0229(17) 0.0127(18)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C8 1.362(6) . ?
O1 C1 1.330(7) . ?
O1 H1 0.8200 . ?
O2 C1 1.199(7) . ?
O3 C3 1.270(6) . ?
O4 C11A 1.365(12) . ?
O4 C10 1.368(6) . ?
O4 C11B 1.408(13) . ?
N1 C6 1.340(7) . ?
N1 C5 1.404(7) . ?
N1 C12B 1.494(13) . ?
N1 C12A 1.501(12) . ?
N2 C9 1.393(7) . ?
N2 C17 1.445(7) . ?
N2 C14 1.458(7) . ?
N3 C15 1.481(8) . ?
N3 C16 1.487(7) . ?
N3 C18 1.488(7) . ?
N3 H3 0.93(6) . ?
C1 C2 1.485(8) . ?
C2 C6 1.350(8) . ?
C2 C3 1.434(8) . ?
C3 C4 1.442(7) . ?
C4 C5 1.405(7) . ?
C4 C7 1.416(8) . ?
C5 C10 1.397(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.337(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.410(8) . ?
C9 C10 1.399(8) . ?
C11A C12A 1.506(15) . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
C12A C13A 1.512(15) . ?
C12A H12A 0.9800 . ?
C13A H13A 0.9600 . ?
C13A H13B 0.9600 . ?
C13A H13C 0.9600 . ?
C11B C12B 1.485(17) . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
C12B C13B 1.516(17) . ?
C12B H12B 0.9800 . ?
C13B H13D 0.9600 . ?
C13B H13E 0.9600 . ?
C13B H13F 0.9600 . ?
C14 C15 1.503(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.500(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O5 C19 1.286(9) . ?
O6 C19 1.246(9) . ?
C19 C20B 1.441(12) . ?
C19 C20A 1.522(11) . ?
O7A C21A 1.352(12) . ?
O7A H7A 0.8200 . ?
O8A C25A 1.318(11) . ?
O8A H8A 0.8200 . ?
C20A C21A 1.3900 . ?
C20A C25A 1.3900 . ?
C21A C22A 1.3900 . ?
C22A C23A 1.3900 . ?
C22A H22A 0.9300 . ?
C23A C24A 1.3900 . ?
C23A H23A 0.9300 . ?
C24A C25A 1.3900 . ?
C24A H24A 0.9300 . ?
O7B C21B 1.347(13) . ?
O7B H7B 0.8200 . ?
O8B C25B 1.384(13) . ?
O8B H8B 0.8200 . ?
C20B C21B 1.3900 . ?
C20B C25B 1.3900 . ?
C21B C22B 1.3900 . ?
C22B C23B 1.3900 . ?
C22B H22B 0.9300 . ?
C23B C24B 1.3900 . ?
C23B H23B 0.9300 . ?
C24B C25B 1.3900 . ?
C24B H24B 0.9300 . ?
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
C1 O1 H1 109.5 . . ?
C11A O4 C10 115.7(8) . . ?
C10 O4 C11B 114.9(8) . . ?
C6 N1 C5 118.4(5) . . ?
C6 N1 C12B 121.5(6) . . ?
C5 N1 C12B 117.4(6) . . ?
C6 N1 C12A 121.9(6) . . ?
C5 N1 C12A 118.6(6) . . ?
C9 N2 C17 124.4(5) . . ?
C9 N2 C14 122.2(5) . . ?
C17 N2 C14 112.0(5) . . ?
C15 N3 C16 111.7(5) . . ?
C15 N3 C18 112.1(5) . . ?
C16 N3 C18 111.3(5) . . ?
C15 N3 H3 118(4) . . ?
C16 N3 H3 105(4) . . ?
C18 N3 H3 98(4) . . ?
O2 C1 O1 121.1(6) . . ?
O2 C1 C2 124.2(6) . . ?
O1 C1 C2 114.6(6) . . ?
C6 C2 C3 119.4(5) . . ?
C6 C2 C1 118.2(5) . . ?
C3 C2 C1 122.5(5) . . ?
O3 C3 C2 122.4(5) . . ?
O3 C3 C4 121.4(5) . . ?
C2 C3 C4 116.1(5) . . ?
C5 C4 C7 118.2(5) . . ?
C5 C4 C3 121.0(5) . . ?
C7 C4 C3 120.8(5) . . ?
C10 C5 N1 119.9(5) . . ?
C10 C5 C4 120.6(5) . . ?
N1 C5 C4 119.5(5) . . ?
N1 C6 C2 125.6(6) . . ?
N1 C6 H6 117.2 . . ?
C2 C6 H6 117.2 . . ?
C8 C7 C4 119.2(6) . . ?
C8 C7 H7 120.4 . . ?
C4 C7 H7 120.4 . . ?
C7 C8 F1 118.9(6) . . ?
C7 C8 C9 125.1(5) . . ?
F1 C8 C9 115.9(5) . . ?
N2 C9 C10 122.2(5) . . ?
N2 C9 C8 122.2(5) . . ?
C10 C9 C8 115.6(5) . . ?
O4 C10 C5 121.0(5) . . ?
O4 C10 C9 117.9(5) . . ?
C5 C10 C9 121.1(5) . . ?
O4 C11A C12A 115.2(10) . . ?
O4 C11A H11A 108.5 . . ?
C12A C11A H11A 108.5 . . ?
O4 C11A H11B 108.5 . . ?
C12A C11A H11B 108.5 . . ?
H11A C11A H11B 107.5 . . ?
N1 C12A C11A 107.8(11) . . ?
N1 C12A C13A 113.0(13) . . ?
C11A C12A C13A 107.3(13) . . ?
N1 C12A H12A 109.6 . . ?
C11A C12A H12A 109.6 . . ?
C13A C12A H12A 109.6 . . ?
C12A C13A H13A 109.5 . . ?
C12A C13A H13B 109.5 . . ?
H13A C13A H13B 109.5 . . ?
C12A C13A H13C 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
O4 C11B C12B 118.4(13) . . ?
O4 C11B H11C 107.7 . . ?
C12B C11B H11C 107.7 . . ?
O4 C11B H11D 107.7 . . ?
C12B C11B H11D 107.7 . . ?
H11C C11B H11D 107.1 . . ?
C11B C12B N1 102.0(13) . . ?
C11B C12B C13B 109.3(16) . . ?
N1 C12B C13B 108.3(13) . . ?
C11B C12B H12B 112.2 . . ?
N1 C12B H12B 112.2 . . ?
C13B C12B H12B 112.2 . . ?
C12B C13B H13D 109.5 . . ?
C12B C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C12B C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
N2 C14 C15 109.2(5) . . ?
N2 C14 H14A 109.8 . . ?
C15 C14 H14A 109.8 . . ?
N2 C14 H14B 109.8 . . ?
C15 C14 H14B 109.8 . . ?
H14A C14 H14B 108.3 . . ?
N3 C15 C14 110.5(5) . . ?
N3 C15 H15A 109.6 . . ?
C14 C15 H15A 109.6 . . ?
N3 C15 H15B 109.6 . . ?
C14 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
N3 C16 C17 110.8(5) . . ?
N3 C16 H16A 109.5 . . ?
C17 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
N2 C17 C16 110.0(5) . . ?
N2 C17 H17A 109.7 . . ?
C16 C17 H17A 109.7 . . ?
N2 C17 H17B 109.7 . . ?
C16 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
N3 C18 H18A 109.5 . . ?
N3 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N3 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O6 C19 O5 121.9(8) . . ?
O6 C19 C20B 120.5(11) . . ?
O5 C19 C20B 117.5(11) . . ?
O6 C19 C20A 121.8(9) . . ?
O5 C19 C20A 116.3(10) . . ?
C21A O7A H7A 109.5 . . ?
C25A O8A H8A 109.5 . . ?
C21A C20A C25A 120.0 . . ?
C21A C20A C19 122.7(11) . . ?
C25A C20A C19 116.9(11) . . ?
O7A C21A C20A 118.8(10) . . ?
O7A C21A C22A 120.9(10) . . ?
C20A C21A C22A 120.0 . . ?
C21A C22A C23A 120.0 . . ?
C21A C22A H22A 120.0 . . ?
C23A C22A H22A 120.0 . . ?
C24A C23A C22A 120.0 . . ?
C24A C23A H23A 120.0 . . ?
C22A C23A H23A 120.0 . . ?
C25A C24A C23A 120.0 . . ?
C25A C24A H24A 120.0 . . ?
C23A C24A H24A 120.0 . . ?
O8A C25A C24A 110.4(12) . . ?
O8A C25A C20A 128.6(12) . . ?
C24A C25A C20A 120.0 . . ?
C21B O7B H7B 109.5 . . ?
C25B O8B H8B 109.5 . . ?
C21B C20B C25B 120.0 . . ?
C21B C20B C19 115.1(13) . . ?
C25B C20B C19 124.8(13) . . ?
O7B C21B C20B 123.4(12) . . ?
O7B C21B C22B 115.2(12) . . ?
C20B C21B C22B 120.0 . . ?
C21B C22B C23B 120.0 . . ?
C21B C22B H22B 120.0 . . ?
C23B C22B H22B 120.0 . . ?
C24B C23B C22B 120.0 . . ?
C24B C23B H23B 120.0 . . ?
C22B C23B H23B 120.0 . . ?
C23B C24B C25B 120.0 . . ?
C23B C24B H24B 120.0 . . ?
C25B C24B H24B 120.0 . . ?
O8B C25B C24B 123.8(14) . . ?
O8B C25B C20B 115.7(14) . . ?
C24B C25B C20B 120.0 . . ?
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
O2 C1 C2 C6 -2.1(9) . . . . ?
O1 C1 C2 C6 177.9(5) . . . . ?
O2 C1 C2 C3 177.2(6) . . . . ?
O1 C1 C2 C3 -2.8(8) . . . . ?
C6 C2 C3 O3 179.3(5) . . . . ?
C1 C2 C3 O3 0.0(8) . . . . ?
C6 C2 C3 C4 0.1(7) . . . . ?
C1 C2 C3 C4 -179.2(5) . . . . ?
O3 C3 C4 C5 179.0(5) . . . . ?
C2 C3 C4 C5 -1.8(7) . . . . ?
O3 C3 C4 C7 0.9(8) . . . . ?
C2 C3 C4 C7 -179.9(5) . . . . ?
C6 N1 C5 C10 177.8(6) . . . . ?
C12B N1 C5 C10 -20.3(11) . . . . ?
C12A N1 C5 C10 9.5(10) . . . . ?
C6 N1 C5 C4 -0.9(8) . . . . ?
C12B N1 C5 C4 161.0(9) . . . . ?
C12A N1 C5 C4 -169.2(8) . . . . ?
C7 C4 C5 C10 1.7(8) . . . . ?
C3 C4 C5 C10 -176.5(5) . . . . ?
C7 C4 C5 N1 -179.7(5) . . . . ?
C3 C4 C5 N1 2.2(8) . . . . ?
C5 N1 C6 C2 -0.9(9) . . . . ?
C12B N1 C6 C2 -162.1(10) . . . . ?
C12A N1 C6 C2 166.9(9) . . . . ?
C3 C2 C6 N1 1.3(9) . . . . ?
C1 C2 C6 N1 -179.4(6) . . . . ?
C5 C4 C7 C8 1.4(8) . . . . ?
C3 C4 C7 C8 179.6(5) . . . . ?
C4 C7 C8 F1 175.2(5) . . . . ?
C4 C7 C8 C9 -1.5(9) . . . . ?
C17 N2 C9 C10 31.3(9) . . . . ?
C14 N2 C9 C10 -134.3(6) . . . . ?
C17 N2 C9 C8 -147.1(6) . . . . ?
C14 N2 C9 C8 47.3(9) . . . . ?
C7 C8 C9 N2 176.8(6) . . . . ?
F1 C8 C9 N2 0.0(8) . . . . ?
C7 C8 C9 C10 -1.6(9) . . . . ?
F1 C8 C9 C10 -178.4(5) . . . . ?
C11A O4 C10 C5 25.4(11) . . . . ?
C11B O4 C10 C5 -4.1(11) . . . . ?
C11A O4 C10 C9 -155.7(9) . . . . ?
C11B O4 C10 C9 174.8(9) . . . . ?
N1 C5 C10 O4 -4.7(8) . . . . ?
C4 C5 C10 O4 173.9(5) . . . . ?
N1 C5 C10 C9 176.4(5) . . . . ?
C4 C5 C10 C9 -4.9(8) . . . . ?
N2 C9 C10 O4 7.4(9) . . . . ?
C8 C9 C10 O4 -174.1(5) . . . . ?
N2 C9 C10 C5 -173.7(6) . . . . ?
C8 C9 C10 C5 4.7(8) . . . . ?
C10 O4 C11A C12A -50.5(19) . . . . ?
C6 N1 C12A C11A 161.4(10) . . . . ?
C5 N1 C12A C11A -30.8(16) . . . . ?
C6 N1 C12A C13A 43.0(17) . . . . ?
C5 N1 C12A C13A -149.1(11) . . . . ?
O4 C11A C12A N1 52(2) . . . . ?
O4 C11A C12A C13A 173.7(11) . . . . ?
C10 O4 C11B C12B 39(2) . . . . ?
O4 C11B C12B N1 -58(2) . . . . ?
O4 C11B C12B C13B -172.9(11) . . . . ?
C6 N1 C12B C11B -151.6(10) . . . . ?
C5 N1 C12B C11B 47.1(15) . . . . ?
C6 N1 C12B C13B -36.4(18) . . . . ?
C5 N1 C12B C13B 162.3(12) . . . . ?
C9 N2 C14 C15 -132.2(6) . . . . ?
C17 N2 C14 C15 60.6(8) . . . . ?
C16 N3 C15 C14 54.4(7) . . . . ?
C18 N3 C15 C14 -179.8(6) . . . . ?
N2 C14 C15 N3 -56.8(8) . . . . ?
C15 N3 C16 C17 -53.5(7) . . . . ?
C18 N3 C16 C17 -179.7(5) . . . . ?
C9 N2 C17 C16 133.2(6) . . . . ?
C14 N2 C17 C16 -59.9(7) . . . . ?
N3 C16 C17 N2 55.2(7) . . . . ?
O6 C19 C20A C21A 0.6(18) . . . . ?
O5 C19 C20A C21A 179.8(9) . . . . ?
O6 C19 C20A C25A -172.3(9) . . . . ?
O5 C19 C20A C25A 7.0(15) . . . . ?
C25A C20A C21A O7A -174.1(16) . . . . ?
C19 C20A C21A O7A 13.2(15) . . . . ?
C25A C20A C21A C22A 0.0 . . . . ?
C19 C20A C21A C22A -172.6(18) . . . . ?
O7A C21A C22A C23A 174.0(16) . . . . ?
C20A C21A C22A C23A 0.0 . . . . ?
C21A C22A C23A C24A 0.0 . . . . ?
C22A C23A C24A C25A 0.0 . . . . ?
C23A C24A C25A O8A -169.8(16) . . . . ?
C23A C24A C25A C20A 0.0 . . . . ?
C21A C20A C25A O8A 167.7(19) . . . . ?
C19 C20A C25A O8A -19.3(16) . . . . ?
C21A C20A C25A C24A 0.0 . . . . ?
C19 C20A C25A C24A 173.0(17) . . . . ?
O6 C19 C20B C21B 6.7(19) . . . . ?
O5 C19 C20B C21B -177.1(9) . . . . ?
O6 C19 C20B C25B -176.8(10) . . . . ?
O5 C19 C20B C25B -1(2) . . . . ?
C25B C20B C21B O7B 166(2) . . . . ?
C19 C20B C21B O7B -17.6(18) . . . . ?
C25B C20B C21B C22B 0.0 . . . . ?
C19 C20B C21B C22B 177(2) . . . . ?
O7B C21B C22B C23B -166.8(19) . . . . ?
C20B C21B C22B C23B 0.0 . . . . ?
C21B C22B C23B C24B 0.0 . . . . ?
C22B C23B C24B C25B 0.0 . . . . ?
C23B C24B C25B O8B 171(2) . . . . ?
C23B C24B C25B C20B 0.0 . . . . ?
C21B C20B C25B O8B -172.1(19) . . . . ?
C19 C20B C25B O8B 11.5(18) . . . . ?
C21B C20B C25B C24B 0.0 . . . . ?
C19 C20B C25B C24B -176(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
O1 H1 O3 0.82 1.80 2.548(6) 150.7 .
N3 H3 O5 0.93(6) 1.76(6) 2.633(7) 156(6) 2_766
C13A H13B O6 0.96 2.64 3.588(17) 170.1 2_765
C13A H13C O7A 0.96 2.58 3.50(2) 159.0 .
C11B H11C O3 0.97 2.53 3.392(19) 147.5 2_755
C12B H12B O3 0.98 2.61 3.461(18) 144.7 2_655
C14 H14B F1 0.97 2.28 2.825(8) 114.9 .
C14 H14B O2 0.97 2.64 3.289(7) 124.7 2_755
C16 H16A O8B 0.97 2.63 3.513(16) 152.0 2_666
C18 H18A F1 0.96 2.60 3.183(8) 119.7 2_656
C18 H18C O2 0.96 2.56 3.432(9) 151.5 1_556
O7A H7A O6 0.82 1.99 2.657(12) 137.6 .
O8A H8A O5 0.82 1.93 2.570(18) 134.1 .
C24A H24A O8A 0.93 2.60 3.383(19) 142.7 2_666
O8B H8B O5 0.82 1.92 2.48(2) 124.7 .
_refine_diff_density_max 0.350
_refine_diff_density_min -0.385
_refine_diff_density_rms 0.064
_shelx_res_file
;
shelx.res created by SHELXL-2014/7
TITL L26AIOU_0m in P-1 white needle
CELL 0.71073 7.0037 12.7637 13.9095 104.821 92.039 95.334
ZERR 2.00 0.0008 0.0028 0.0031 0.004 0.004 0.004
LATT 1
SFAC C H N O F
UNIT 50 52 6 16 2
L.S. 30
ACTA 52
BOND $H
HTAB
CONF
LIST 4
FMAP 2
PLAN 20
TEMP 23.000
size 0.40 0.22 0.18
DFIX 1.40 N1 C12A N1 C12B
DFIX 1.45 O4 C11A O4 C11B
DFIX 1.50 C11A C12A C11B C12B C12A C13A C12B C13B
EADP C11A C12A C11B C12B C13A C13B
EADP C20A C21A C22A C23A C24A C25A C20B C21B C22B C23B C24B C25B O7A O8A =
O7B O8B
DFIX 1.3 C21A O7A C21B O7B C25A O8A C25B O8B
DFIX 1.45 C19 C20A C19 C20B
HTAB O1 O3
EQIV $1 -x+2, -y+1, -z+1
HTAB N3 O5_$1
EQIV $2 -x+2, -y+1, -z
HTAB C13A O6_$2
HTAB C13A O7A
EQIV $3 -x+2, -y, -z
HTAB C11B O3_$3
EQIV $4 -x+1, -y, -z
HTAB C12B O3_$4
HTAB C14 F1
HTAB C14 O2_$3
EQIV $5 -x+1, -y+1, -z+1
HTAB C16 O8B_$5
EQIV $6 -x+1, -y, -z+1
HTAB C18 F1_$6
EQIV $7 x, y, z+1
HTAB C18 O2_$7
HTAB O7A O6
HTAB O8A O5
HTAB C24A O8A_$5
HTAB O8B O5
OMIT 1 1 0
WGHT 0.000000 5.308900
EXTI 0.004776
FVAR 0.60303 0.54134 0.49770
F1 5 0.738898 -0.076753 0.285251 11.00000 0.10424 0.06755 =
0.06056 0.03635 0.03085 0.02066
O1 4 0.705778 -0.176485 -0.269082 11.00000 0.07304 0.06222 =
0.04996 -0.00448 -0.00848 0.01412
AFIX 147
H1 2 0.724152 -0.199336 -0.219900 11.00000 -1.50000
AFIX 0
O2 4 0.720732 -0.016564 -0.302955 11.00000 0.08821 0.08255 =
0.04134 0.01787 0.00435 0.01976
O3 4 0.707779 -0.187252 -0.088625 11.00000 0.05496 0.04218 =
0.06278 0.00372 0.00270 0.00236
O4 4 0.847653 0.257052 0.198824 11.00000 0.09711 0.04265 =
0.04055 0.00682 0.00271 -0.00208
N1 3 0.781332 0.147500 -0.003425 11.00000 0.07804 0.03812 =
0.03876 0.00813 0.00281 0.01265
N2 3 0.794777 0.147001 0.346347 11.00000 0.07704 0.06359 =
0.03487 0.01339 0.00969 0.03483
N3 3 0.714382 0.215180 0.549256 11.00000 0.05176 0.05387 =
0.03815 0.01516 0.01400 0.01642
H3 2 0.800512 0.274964 0.580069 11.00000 -1.20000
C1 1 0.721393 -0.068120 -0.242003 11.00000 0.03553 0.05610 =
0.04707 -0.00265 0.00187 0.01441
C2 1 0.739025 -0.019087 -0.132628 11.00000 0.02897 0.04469 =
0.04230 0.00652 0.00085 0.00902
C3 1 0.730737 -0.083756 -0.062128 11.00000 0.01929 0.04563 =
0.05199 0.00632 0.00147 0.00513
C4 1 0.747533 -0.024534 0.041569 11.00000 0.02543 0.04409 =
0.04597 0.01438 0.00852 0.00208
C5 1 0.775876 0.089912 0.070148 11.00000 0.03581 0.04407 =
0.03386 0.01383 0.00653 0.00536
C6 1 0.761607 0.090665 -0.099287 11.00000 0.05218 0.05326 =
0.04032 0.01460 0.00414 0.00828
AFIX 43
H6 2 0.763649 0.130218 -0.146939 11.00000 -1.20000
AFIX 0
C7 1 0.741597 -0.080443 0.117338 11.00000 0.03663 0.04051 =
0.05168 0.01019 0.01224 0.01081
AFIX 43
H7 2 0.725934 -0.156208 0.100974 11.00000 -1.20000
AFIX 0
C8 1 0.758801 -0.022922 0.212740 11.00000 0.04146 0.05611 =
0.04981 0.02350 0.01966 0.01450
C9 1 0.787263 0.091739 0.245766 11.00000 0.04383 0.04666 =
0.04276 0.01278 0.00616 0.01297
C10 1 0.802503 0.146487 0.170705 11.00000 0.05109 0.03465 =
0.04314 0.00715 0.00672 0.00535
PART 1
C11A 1 0.790656 0.311794 0.132174 21.00000 0.09170 0.04399 =
0.04821 0.01011 0.01259 0.02054
AFIX 23
H11A 2 0.845024 0.387251 0.155434 21.00000 -1.20000
H11B 2 0.651950 0.310827 0.131326 21.00000 -1.20000
AFIX 0
C12A 1 0.846482 0.267338 0.027090 21.00000 0.09170 0.04399 =
0.04821 0.01011 0.01259 0.02054
AFIX 13
H12A 2 0.986400 0.278699 0.024836 21.00000 -1.20000
AFIX 0
C13A 1 0.752416 0.329794 -0.037041 21.00000 0.09170 0.04399 =
0.04821 0.01011 0.01259 0.02054
AFIX 137
H13A 2 0.618241 0.304196 -0.049094 21.00000 -1.50000
H13B 2 0.812260 0.318815 -0.099372 21.00000 -1.50000
H13C 2 0.767004 0.406036 -0.003388 21.00000 -1.50000
AFIX 0
PART 2
C11B 1 0.876998 0.305807 0.119702 -21.00000 0.09170 0.04399 =
0.04821 0.01011 0.01259 0.02054
AFIX 23
H11C 2 1.008172 0.298314 0.101073 -21.00000 -1.20000
H11D 2 0.866389 0.383131 0.144891 -21.00000 -1.20000
AFIX 0
C12B 1 0.749023 0.265163 0.027652 -21.00000 0.09170 0.04399 =
0.04821 0.01011 0.01259 0.02054
AFIX 13
H12B 2 0.614284 0.275379 0.040089 -21.00000 -1.20000
AFIX 0
C13B 1 0.821815 0.318815 -0.051368 -21.00000 0.09170 0.04399 =
0.04821 0.01011 0.01259 0.02054
AFIX 137
H13D 2 0.816847 0.396107 -0.028877 -21.00000 -1.50000
H13E 2 0.742685 0.290267 -0.111924 -21.00000 -1.50000
H13F 2 0.952022 0.304055 -0.063356 -21.00000 -1.50000
AFIX 0
PART 0
C14 1 0.910802 0.115640 0.421489 11.00000 0.05631 0.08483 =
0.03987 0.02061 0.00995 0.03751
AFIX 23
H14A 2 1.022100 0.168745 0.443997 11.00000 -1.20000
H14B 2 0.955567 0.045269 0.393060 11.00000 -1.20000
AFIX 0
C15 1 0.791385 0.109763 0.507995 11.00000 0.08684 0.07534 =
0.05067 0.02806 0.02523 0.03706
AFIX 23
H15A 2 0.685892 0.052588 0.486233 11.00000 -1.20000
H15B 2 0.869466 0.091928 0.559409 11.00000 -1.20000
AFIX 0
C16 1 0.606901 0.250965 0.471230 11.00000 0.04702 0.05171 =
0.04857 0.00834 0.00404 0.01512
AFIX 23
H16A 2 0.569702 0.323328 0.499303 11.00000 -1.20000
H16B 2 0.490820 0.201728 0.448510 11.00000 -1.20000
AFIX 0
C17 1 0.727552 0.252491 0.384564 11.00000 0.06518 0.05238 =
0.03976 0.01318 0.00328 0.02139
AFIX 23
H17A 2 0.652222 0.270900 0.332500 11.00000 -1.20000
H17B 2 0.836527 0.307540 0.405542 11.00000 -1.20000
AFIX 0
C18 1 0.595614 0.212801 0.635404 11.00000 0.08757 0.08562 =
0.06933 0.03123 0.04143 0.02889
AFIX 137
H18A 2 0.466761 0.182640 0.611524 11.00000 -1.50000
H18B 2 0.594095 0.285596 0.676597 11.00000 -1.50000
H18C 2 0.649350 0.168633 0.673677 11.00000 -1.50000
AFIX 0
MOLE 2
O5 4 0.976454 0.644888 0.394838 11.00000 0.06934 0.11321 =
0.06397 0.01090 -0.01741 -0.01188
O6 4 0.971016 0.691581 0.252157 11.00000 0.09957 0.14016 =
0.09168 0.04113 0.00538 0.00166
C19 1 0.897842 0.639359 0.308491 11.00000 0.08493 0.08159 =
0.06420 0.00360 -0.00039 0.02198
PART 1
O7A 4 0.695690 0.587682 0.115629 21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
AFIX 147
H7A 2 0.810226 0.604880 0.132047 21.00000 -1.50000
AFIX 0
O8A 4 0.712275 0.511507 0.434962 21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
AFIX 147
H8A 2 0.796757 0.561984 0.456404 21.00000 -1.50000
AFIX 66
C20A 1 0.709099 0.566578 0.279366 21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
C21A 1 0.607676 0.552951 0.188526 21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
C22A 1 0.425748 0.495600 0.170672 21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
AFIX 43
H22A 2 0.357890 0.486482 0.109894 21.00000 -1.20000
AFIX 65
C23A 1 0.345243 0.451875 0.243658 21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
AFIX 43
H23A 2 0.223521 0.413503 0.231712 21.00000 -1.20000
AFIX 65
C24A 1 0.446664 0.465502 0.334498 21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
AFIX 43
H24A 2 0.392799 0.436247 0.383331 21.00000 -1.20000
AFIX 65
C25A 1 0.628592 0.522853 0.352354 21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
PART 0
AFIX 0
PART 2
O7B 4 0.701795 0.636529 0.130960 -21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
AFIX 147
H7B 2 0.815284 0.630594 0.120517 -21.00000 -1.50000
AFIX 0
O8B 4 0.688458 0.541951 0.438654 -21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
AFIX 147
H8B 2 0.747716 0.602937 0.454440 -21.00000 -1.50000
AFIX 66
C20B 1 0.714117 0.575463 0.281041 -21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
C21B 1 0.639853 0.568004 0.185233 -21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
C22B 1 0.468198 0.503859 0.149049 -21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
AFIX 43
H22B 2 0.418511 0.498869 0.084947 -21.00000 -1.20000
AFIX 65
C23B 1 0.370804 0.447172 0.208674 -21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
AFIX 43
H23B 2 0.255955 0.404255 0.184464 -21.00000 -1.20000
AFIX 65
C24B 1 0.445066 0.454630 0.304482 -21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
AFIX 43
H24B 2 0.379903 0.416702 0.344375 -21.00000 -1.20000
AFIX 65
C25B 1 0.616721 0.518774 0.340666 -21.00000 0.09251 0.05630 =
0.07310 0.00676 -0.02287 0.01269
AFIX 0
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM L26AIOU_0m in P-1 white needle
REM R1 = 0.1121 for 2383 Fo > 4sig(Fo) and 0.2040 for all 5139 data
REM 303 parameters refined using 14 restraints
END
WGHT 0.0000 5.3132
REM Instructions for potential hydrogen bonds
HTAB O1 O3
HTAB N3 O5_$1
HTAB C13A O6_$2
HTAB C13A O7A
HTAB C11B O3_$3
HTAB C12B O3_$4
HTAB C14 F1
HTAB C14 O2_$3
HTAB C16 O8B_$5
HTAB C18 F1_$6
HTAB C18 O2_$7
HTAB O7A O6
HTAB O8A O5
HTAB C24A O8A_$5
HTAB O8B O5
REM Highest difference peak 0.350, deepest hole -0.385, 1-sigma level 0.064
Q1 1 0.4359 0.4532 0.1600 11.00000 0.05 0.31
Q2 1 0.7107 0.0999 0.7334 11.00000 0.05 0.26
Q3 1 0.6830 0.0300 0.0415 11.00000 0.05 0.24
Q4 1 0.6078 0.4976 0.3542 11.00000 0.05 0.23
Q5 1 0.2967 0.4867 0.3141 11.00000 0.05 0.23
Q6 1 1.0711 0.5589 0.2650 11.00000 0.05 0.22
Q7 1 0.9104 0.5770 0.5452 11.00000 0.05 0.22
Q8 1 1.0134 0.2492 0.4594 11.00000 0.05 0.22
Q9 1 0.7235 -0.0462 -0.0103 11.00000 0.05 0.22
Q10 1 0.8466 0.2879 0.1606 11.00000 0.05 0.21
Q11 1 0.7029 -0.1726 -0.0060 11.00000 0.05 0.21
Q12 1 0.4315 0.2835 0.6569 11.00000 0.05 0.21
Q13 1 0.9513 0.2343 0.6012 11.00000 0.05 0.21
Q14 1 0.7215 0.2203 0.1912 11.00000 0.05 0.20
Q15 1 0.4999 0.4864 0.0860 11.00000 0.05 0.20
Q16 1 0.6910 -0.1154 -0.3795 11.00000 0.05 0.20
Q17 1 1.0338 -0.0125 0.3238 11.00000 0.05 0.20
Q18 1 0.8082 0.1106 0.0374 11.00000 0.05 0.19
Q19 1 0.3046 0.5735 0.3579 11.00000 0.05 0.19
Q20 1 0.8589 0.3381 0.5071 11.00000 0.05 0.19
;
_shelx_res_checksum 90650
_shelx_hkl_file
;
-1 0 0 7.78089 2.77071 3
-1 0 0 10.7198 2.6034 4
1 0 0 19.3367 2.7057 4
1 0 0 12.3112 2.4056 5
-2 0 0 8930.55 560.13 3
2 0 0 9999.99 551.14 4
2 0 0 9149.56 570.99 5
-3 0 0 345.324 24.087 3
3 0 0 363.737 23.560 4
3 0 0 347.625 23.709 5
-4 0 0 952.906 61.434 3
4 0 0 969.415 61.579 5
-5 0 0 12.8955 5.2745 3
5 0 0 11.7546 3.6878 5
-6 0 0 121.202 14.903 3
6 0 0 101.946 11.857 5
-7 0 0 21.9144 8.3888 3
7 0 0 13.0980 5.3068 5
-8 0 0 0.11770 7.09238 3
-8 1 0 14.9819 8.4064 3
7 -1 0 -1.4176 3.5804 5
-7 1 0 6.42096 6.74382 3
6 -1 0 248.564 20.342 5
-6 1 0 298.565 23.131 3
5 -1 0 8.88030 3.11812 5
-5 1 0 6.63362 4.57173 3
4 -1 0 2536.82 156.92 5
-4 1 0 2529.75 155.19 3
3 -1 0 130.395 9.806 5
3 -1 0 127.119 10.370 4
-3 1 0 125.520 10.607 3
2 -1 0 7899.05 468.73 5
2 -1 0 7268.60 452.66 4
-2 1 0 7897.12 468.78 5
-2 1 0 7772.41 452.80 4
-2 1 0 7570.40 460.09 3
1 -1 0 120.436 7.690 4
1 -1 0 88.3290 7.2454 5
1 -1 0 122.384 7.796 3
-1 1 0 117.919 7.182 1
1 1 0 1165.74 80.65 1
1 1 0 1487.91 80.74 1
-2 -1 0 1476.84 91.25 1
-2 -1 0 1487.71 91.29 1
2 1 0 1538.09 89.63 4
2 1 0 1506.23 91.06 1
2 1 0 1485.65 91.05 1
-3 -1 0 127.473 8.607 1
-3 -1 0 128.757 8.665 1
-3 -1 0 128.876 10.695 3
3 1 0 128.993 10.173 5
3 1 0 108.028 9.932 4
-4 -1 0 20.5989 2.6682 1
-4 -1 0 25.1576 2.8464 1
-4 -1 0 9.44963 4.64749 3
4 1 0 16.9091 3.9252 5
4 1 0 15.3709 3.8080 4
-5 -1 0 45.8987 4.3040 1
-5 -1 0 27.4421 7.2174 3
-5 -1 0 48.6703 4.4332 1
5 1 0 37.4530 6.4412 5
-6 -1 0 11.5501 6.2757 3
6 1 0 11.1054 4.2668 5
-7 -1 0 1.28085 6.33470 3
-8 -1 0 2.47692 6.56542 3
-8 2 0 43.7008 11.4495 3
-7 2 0 8.70200 6.22872 3
6 -2 0 264.091 20.777 5
-6 2 0 308.718 23.827 3
5 -2 0 5.40370 2.61305 5
-5 2 0 8.06954 4.51906 3
4 -2 0 535.508 34.892 5
-4 2 0 530.043 36.015 3
3 -2 0 75.6100 6.3131 5
3 -2 0 82.2170 8.2385 4
-3 2 0 75.8277 8.4811 3
-3 2 0 74.7850 5.5417 1
-3 2 0 83.5050 5.6495 1
-3 2 0 70.9088 6.5081 5
2 -2 0 1205.32 73.90 1
2 -2 0 1242.18 74.81 5
2 -2 0 1240.53 73.20 4
2 -2 0 1255.07 73.92 1
-2 2 0 1187.98 74.12 1
-2 2 0 1163.47 74.08 1
-2 2 0 1242.34 73.27 4
-2 2 0 1184.25 74.12 1
-2 2 0 1201.52 74.88 5
1 -2 0 2578.61 155.39 1
1 -2 0 2636.35 156.14 5
1 -2 0 2656.40 155.44 1
1 -2 0 2522.99 168.88 2
1 -2 0 2584.34 151.12 4
-1 2 0 2543.34 168.74 2
-1 2 0 2284.95 151.07 4
-1 2 0 2584.49 168.75 2
-1 2 0 2584.81 155.46 1
-1 2 0 2582.95 156.15 5
0 -2 0 145.272 10.149 1
0 -2 0 144.737 10.194 1
0 -2 0 147.349 10.130 1
0 -2 0 156.318 8.958 6
0 2 0 151.175 10.180 1
0 2 0 154.111 11.151 2
0 2 0 153.156 10.202 1
-1 -2 0 35.0705 3.6812 1
-1 -2 0 46.7618 4.1866 1
1 2 0 33.0586 3.6074 1
1 2 0 35.2460 3.6569 1
-2 -2 0 77.3676 6.1498 1
2 2 0 69.6604 6.0032 1
2 2 0 86.8650 6.5020 4
2 2 0 82.1941 6.0975 1
-3 -2 0 213.654 17.348 1
3 2 0 275.358 17.166 1
3 2 0 283.050 17.163 1
3 2 0 306.209 18.477 4
-4 -2 0 18.1192 2.8940 1
-4 -2 0 12.0024 2.5276 1
4 2 0 15.2752 3.6837 4
4 2 0 9.89229 3.44001 5
-5 -2 0 7.97161 2.53142 1
-5 -2 0 7.14016 2.27813 1
-5 -2 0 12.0706 5.5041 3
5 2 0 8.83450 3.49273 5
-6 -2 0 11.7821 2.6319 1
-6 -2 0 11.0899 2.8991 1
-6 -2 0 18.7001 6.8729 3
6 2 0 5.26345 3.88515 5
-7 -2 0 2.17334 6.04275 3
-8 -2 0 1.35540 6.76861 3
6 -3 0 128.803 11.388 5
-6 3 0 115.518 14.908 3
5 -3 0 24.7992 4.3394 5
-5 3 0 15.6867 5.4159 3
4 -3 0 283.485 18.924 5
-4 3 0 268.725 19.074 5
-4 3 0 296.939 17.963 1
-4 3 0 251.303 17.750 1
3 -3 0 24.0998 4.5374 4
3 -3 0 33.8422 3.8513 5
3 -3 0 35.4142 3.2546 1
3 -3 0 35.3352 3.1795 1
-3 3 0 27.4232 3.7935 5
-3 3 0 33.3218 3.7755 1
-3 3 0 28.5719 4.8641 4
-3 3 0 35.7556 3.8755 1
2 -3 0 507.871 31.297 5
2 -3 0 496.226 33.682 2
2 -3 0 484.012 31.269 1
2 -3 0 507.157 33.705 2
2 -3 0 505.090 31.345 1
2 -3 0 530.125 31.450 4
-2 3 0 484.336 31.418 4
-2 3 0 517.877 31.568 1
-2 3 0 455.117 31.359 5
1 -3 0 7272.30 447.82 1
1 -3 0 7677.95 487.27 2
1 -3 0 7362.94 434.60 4
1 -3 0 7456.65 447.78 1
-1 3 0 6935.17 434.65 4
-1 3 0 7542.13 447.88 1
-1 3 0 7451.84 447.83 1
0 -3 0 199.140 14.117 1
0 -3 0 211.995 12.409 6
0 -3 0 210.424 14.204 1
0 -3 0 213.401 14.310 1
0 3 0 197.673 12.660 4
0 3 0 208.332 14.164 1
0 3 0 233.666 15.988 2
0 3 0 209.442 14.240 1
0 3 0 202.859 12.476 6
-1 -3 0 244.834 16.660 1
-1 -3 0 248.760 16.759 1
1 3 0 246.525 16.605 1
1 3 0 246.738 16.579 1
-2 -3 0 1242.26 77.40 1
-2 -3 0 1281.67 77.52 1
2 3 0 1281.97 77.34 1
2 3 0 1254.36 74.85 4
2 3 0 1191.86 77.12 1
-3 -3 0 39.1527 4.8856 1
-3 -3 0 42.5912 5.1826 1
-3 -3 0 42.1620 5.0485 1
3 3 0 50.6706 5.0928 1
3 3 0 35.2181 4.8134 4
3 3 0 39.0770 4.5503 1
-4 -3 0 1.05675 1.49688 1
-4 -3 0 12.1196 2.9305 1
4 3 0 3.15065 2.47203 5
4 3 0 6.91090 1.84162 1
4 3 0 12.4463 3.4791 4
-5 -3 0 17.3323 6.0953 3
-5 -3 0 10.3956 3.2727 1
-5 -3 0 12.4216 3.1328 1
5 3 0 16.9932 4.6711 5
-6 -3 0 21.0172 7.5277 3
-6 -3 0 21.1321 3.9344 1
-7 -3 0 21.9184 4.2428 1
-7 -3 0 20.1136 8.4467 3
-8 -3 0 4.38122 7.88948 3
6 -4 0 7.44866 3.03805 5
-6 4 0 7.31658 2.32195 1
-6 4 0 5.15477 1.81450 1
5 -4 0 38.2368 4.8914 5
-5 4 0 28.9149 4.8635 5
-5 4 0 31.3184 4.1870 1
-5 4 0 26.3944 3.6956 1
4 -4 0 15.1813 2.8959 5
-4 4 0 26.0250 3.4884 1
-4 4 0 21.0250 3.4064 1
-4 4 0 15.0763 3.2900 5
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