data_fasac13
_vrf_STRVA01_fasac13
;
PROBLEM: _C Flack parameter is too small
From the CIF: _refine_ls_abs_structure_Flack -0.300
From the CIF: _refine_ls_abs_structure_Flack_su 0.300
RESPONSE: Although the Flack parameter is small and its standard
uncertainty has a large range, the inverted structure's Flack
parameter refines to above 1. Additionally, the crystal was a pure
enantiomer from a sample of known stereochemistry.
;
_vrf_PLAT032_fasac13
;
PROBLEM: _G Std. Uncertainty on Flack Parameter Value High .. 0.300
RESPONSE: See above.
;
_audit_creation_date 2019-08-22
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number '2018/3'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
#CrysAlisPro, version 171.40.58a
Rigaku Oxford Diffraction (2019). CrysAlisPro Software system,
version 171.40.58a. Rigaku Corporation, Oxford, UK.
#SHELXT-2018/2
Sheldrick, G. M. (2015a). Acta Cryst. A71, 3--8.
#SHELXL-2018/3
Sheldrick, G. M. (2015b). Acta Cryst. C71, 3--8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C12 H13 N O'
_chemical_formula_sum 'C12 H13 N O'
_chemical_formula_weight 187.23
_chemical_absolute_configuration ad
_chemical_melting_point ?
_chemical_oxdiff_formula ?
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'
'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 'monoclinic'
_space_group_IT_number 4
_space_group_name_H-M_alt 'P 1 21 1'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 5.6803(2)
_cell_length_b 9.2798(3)
_cell_length_c 9.3092(3)
_cell_angle_alpha 90
_cell_angle_beta 90.739(3)
_cell_angle_gamma 90
_cell_volume 490.67(3)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 3711
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 77.2080
_cell_measurement_theta_min 4.7830
_shelx_estimated_absorpt_T_max 0.978
_shelx_estimated_absorpt_T_min 0.913
_exptl_absorpt_coefficient_mu 0.638
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.61067
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.267
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 200
_exptl_crystal_size_max 0.145
_exptl_crystal_size_mid 0.066
_exptl_crystal_size_min 0.035
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0666
_diffrn_reflns_av_unetI/netI 0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 7207
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full 74.504
_diffrn_reflns_theta_max 77.848
_diffrn_reflns_theta_min 4.751
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
--------------------------------------------------------------------------
1 \w -83.00 -47.00 0.50 0.10 -- -49.75 -30.00 -91.00 72
2 \w -75.00 -18.00 0.50 0.10 -- -49.75 98.00-102.00 114
3 \w -20.00 5.00 0.50 0.10 -- 49.75 -30.00 -91.00 50
4 \w 58.00 83.00 0.50 0.10 -- 49.75 30.00 68.00 50
5 \w -143.00-118.00 0.50 0.39 -- -84.25-110.00 61.00 50
6 \w -72.00 -47.00 0.50 0.39 -- -84.25 110.00 157.00 50
7 \w -145.00-120.00 0.50 0.39 -- -84.25 -98.00 150.00 50
8 \w 51.00 98.00 0.50 0.39 -- 105.75 -98.00 150.00 94
9 \w 108.00 158.00 0.50 0.39 -- 105.75 110.00 157.00 100
10 \w 111.00 176.00 0.50 0.39 -- 105.75 30.00 68.00 130
11 \w 122.00 147.00 0.50 0.39 -- 105.75 98.00-102.00 50
12 \w 43.00 70.00 0.50 0.10 -- 49.75 57.00-180.00 54
13 \w 43.00 80.00 0.50 0.10 -- 49.75 38.00 150.00 74
14 \w 41.00 75.00 0.50 0.10 -- 49.75 57.00-150.00 68
15 \w -97.00 -72.00 0.50 0.39 -- -84.25 -61.00-180.00 50
16 \w -99.00 -72.00 0.50 0.39 -- -84.25 -58.00 165.36 54
17 \w -88.00 -63.00 0.50 0.39 -- -84.25 -77.00-180.00 50
18 \w -104.00 -75.00 0.50 0.39 -- -84.25 -61.00 150.00 58
19 \w -151.00-125.00 0.50 0.39 -- -84.25 -30.00 150.00 52
20 \w 68.00 96.00 0.50 0.39 -- 105.75-125.00 150.00 56
21 \w 56.00 81.00 0.50 0.39 -- 105.75 -77.00 -60.00 50
22 \w 36.00 70.00 0.50 0.39 -- 105.75 -61.00 30.00 68
23 \w 90.00 122.00 0.50 0.39 -- 105.75 -77.00 -60.00 64
24 \w 95.00 133.00 0.50 0.39 -- 105.75 61.00-180.00 76
25 \w 94.00 125.00 0.50 0.39 -- 105.75 77.00 150.00 62
26 \w 94.00 142.00 0.50 0.39 -- 105.75 61.00 150.00 96
27 \w 90.00 130.00 0.50 0.39 -- 105.75 77.00 120.00 80
28 \w 43.00 69.00 0.50 0.39 -- 105.75 -61.00-150.00 52
29 \w 25.00 52.00 0.50 0.10 -- 49.87-109.00 61.00 54
30 \w -3.00 24.00 0.50 0.10 -- -49.87 19.00 90.00 54
31 \w -5.00 20.00 0.50 0.10 -- -49.87 19.00 0.00 50
32 \w -112.00 -83.00 0.50 0.10 -- -49.87-125.00 30.00 58
33 \w -4.00 22.00 0.50 0.10 -- -49.87 19.00 120.00 52
34 \w -15.00 13.00 0.50 0.10 -- 49.87 -19.00 150.00 56
35 \w 56.00 81.00 0.50 0.10 -- 49.87-109.00 61.00 50
36 \w 46.00 72.00 0.50 0.10 -- 49.87-125.00-180.00 52
37 \w -20.00 6.00 0.50 0.10 -- 49.87 -19.00 0.00 52
38 \w 37.00 67.00 0.50 0.39 -- 105.75 -61.00 60.00 60
39 \w 35.00 78.00 0.50 0.39 -- 105.75-125.00-150.00 86
40 \w 67.00 104.00 0.50 0.39 -- 105.75 -94.00 -60.00 74
41 \w 80.00 109.00 0.50 0.39 -- 105.75-125.00-150.00 58
42 \w 57.00 104.00 0.50 0.39 -- 105.75 -94.00 90.00 94
43 \w 72.00 105.00 0.50 0.39 -- 105.75 -94.00-120.00 66
44 \w 135.00 176.00 0.50 0.39 -- 105.75 45.00-120.00 82
45 \w 39.00 65.00 0.50 0.39 -- 105.75-125.00-180.00 52
46 \w 34.00 59.00 0.50 0.39 -- 105.75-125.00 30.00 50
47 \w 61.00 87.00 0.50 0.39 -- 105.75 -94.00 60.00 52
48 \w 35.00 64.00 0.50 0.39 -- 105.75 -94.00 -60.00 58
49 \w 79.00 106.00 0.50 0.39 -- 105.75-125.00 30.00 54
50 \w 35.00 64.00 0.50 0.39 -- 105.75 -61.00 90.00 58
51 \w 77.00 111.00 0.50 0.39 -- 105.75-125.00-180.00 68
52 \w 65.00 107.00 0.50 0.39 -- 105.75-109.00 61.00 84
53 \w 97.00 144.00 0.50 0.39 -- 105.75 77.00-180.00 94
54 \w 40.00 66.00 0.50 0.39 -- 105.75 -61.00-120.00 52
55 \w 141.00 166.00 0.50 0.39 -- 105.75 30.00 -90.00 50
56 \w 134.00 172.00 0.50 0.39 -- 105.75 45.00 0.00 76
57 \w 97.00 126.00 0.50 0.39 -- 105.75 45.00 0.00 58
58 \w 34.00 59.00 0.50 0.39 -- 105.75 -61.00 0.00 50
59 \w 101.00 137.00 0.50 0.39 -- 105.75 30.00 -90.00 72
60 \w 98.00 127.00 0.50 0.39 -- 105.75 45.00-120.00 58
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.1085838000
_diffrn_orient_matrix_UB_12 -0.0535869000
_diffrn_orient_matrix_UB_13 -0.1428644000
_diffrn_orient_matrix_UB_21 0.0203034000
_diffrn_orient_matrix_UB_22 0.1529103000
_diffrn_orient_matrix_UB_23 -0.0628771000
_diffrn_orient_matrix_UB_31 0.2477946000
_diffrn_orient_matrix_UB_32 -0.0360347000
_diffrn_orient_matrix_UB_33 -0.0549801000
_diffrn_oxdiff_digest_frames
;
010cda9f0a4ba1ba8acc932fe7dd8e8c9f01874095a
;
_diffrn_oxdiff_digest_hkl
;
018bbef581843999c6ae73f0ec2cee76346d83
;
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage 0.853
_reflns_Friedel_fraction_full 0.988
_reflns_Friedel_fraction_max 0.957
_reflns_number_gt 1854
_reflns_number_total 2033
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 74.33
_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 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max 0.156
_refine_diff_density_min -0.220
_refine_diff_density_rms 0.042
_refine_ls_abs_structure_details
;
Flack x determined using 778 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.3(3)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.057
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 128
_refine_ls_number_reflns 2033
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0482
_refine_ls_R_factor_gt 0.0438
_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^)+(0.0664P)^2^+0.0396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1144
_refine_ls_wR_factor_ref 0.1183
_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 Ternary CH refined with riding coordinates:
C1(H1), C2(H2), C3(H3)
2.b Secondary CH2 refined with riding coordinates:
C4(H4A,H4B)
2.c Aromatic/amide H refined with riding coordinates:
C7(H7), C8(H8), C9(H9), C10(H10), C11(H11)
2.d Idealised Me refined as rotating group:
C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
O1 O 0.9341(5) 0.7499(3) 0.5903(3) 0.0457(6) Uani 1 1 d . . . . .
N1 N 0.8047(4) 0.5839(3) 0.4242(2) 0.0258(5) Uani 1 1 d . . . . .
C1 C 0.5836(4) 0.4501(3) 0.6715(3) 0.0247(5) Uani 1 1 d . . . . .
H1 H 0.735187 0.400837 0.662054 0.030 Uiso 1 1 calc R . . . .
C2 C 0.5794(5) 0.6072(3) 0.6260(3) 0.0303(6) Uani 1 1 d . . . . .
H2 H 0.481740 0.676503 0.677738 0.036 Uiso 1 1 calc R . . . .
C3 C 0.4658(4) 0.4943(4) 0.5333(3) 0.0322(7) Uani 1 1 d . . . . .
H3 H 0.293672 0.490696 0.525425 0.039 Uiso 1 1 calc R . . . .
C4 C 0.6112(5) 0.4846(4) 0.3982(3) 0.0344(7) Uani 1 1 d . . . . .
H4A H 0.668884 0.387288 0.383911 0.041 Uiso 1 1 calc R . . . .
H4B H 0.519402 0.513319 0.314416 0.041 Uiso 1 1 calc R . . . .
C5 C 0.7924(5) 0.6577(3) 0.5486(3) 0.0295(6) Uani 1 1 d . . . . .
C6 C 0.4383(4) 0.4047(3) 0.7953(3) 0.0241(6) Uani 1 1 d . . . . .
C7 C 0.5154(4) 0.2924(3) 0.8837(3) 0.0276(6) Uani 1 1 d . . . . .
H7 H 0.655329 0.245130 0.863302 0.033 Uiso 1 1 calc R . . . .
C8 C 0.3855(5) 0.2506(3) 1.0020(3) 0.0319(6) Uani 1 1 d . . . . .
H8 H 0.439380 0.175311 1.059543 0.038 Uiso 1 1 calc R . . . .
C9 C 0.1771(5) 0.3192(3) 1.0353(3) 0.0300(6) Uani 1 1 d . . . . .
H9 H 0.091777 0.291364 1.115306 0.036 Uiso 1 1 calc R . . . .
C10 C 0.0973(5) 0.4305(3) 0.9472(3) 0.0297(6) Uani 1 1 d . . . . .
H10 H -0.042556 0.477562 0.968561 0.036 Uiso 1 1 calc R . . . .
C11 C 0.2241(4) 0.4720(3) 0.8281(3) 0.0279(6) Uani 1 1 d . . . . .
H11 H 0.166773 0.545210 0.769142 0.033 Uiso 1 1 calc R . . . .
C12 C 0.9886(4) 0.6034(3) 0.3199(3) 0.0292(6) Uani 1 1 d . . . . .
H12A H 1.056021 0.511572 0.296729 0.044 Uiso 1 1 calc GR . . . .
H12B H 1.108495 0.665294 0.359208 0.044 Uiso 1 1 calc GR . . . .
H12C H 0.923161 0.646285 0.234409 0.044 Uiso 1 1 calc GR . . . .
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
O1 0.0680(15) 0.0305(11) 0.0390(12) -0.0066(10) 0.0101(10) -0.0212(11)
N1 0.0284(11) 0.0222(11) 0.0268(11) -0.0007(9) 0.0004(8) -0.0005(9)
C1 0.0217(11) 0.0221(12) 0.0301(12) -0.0005(10) -0.0013(9) 0.0009(10)
C2 0.0366(14) 0.0227(14) 0.0316(14) 0.0031(12) 0.0046(11) 0.0062(11)
C3 0.0222(12) 0.0443(17) 0.0301(14) 0.0011(13) -0.0005(10) -0.0025(12)
C4 0.0283(12) 0.0475(18) 0.0275(13) -0.0024(13) -0.0021(10) -0.0110(12)
C5 0.0402(14) 0.0201(13) 0.0283(13) 0.0012(11) 0.0014(11) -0.0007(12)
C6 0.0242(11) 0.0214(12) 0.0265(13) -0.0023(11) -0.0045(10) -0.0019(10)
C7 0.0260(11) 0.0248(13) 0.0321(14) 0.0005(11) -0.0012(10) 0.0012(11)
C8 0.0366(14) 0.0267(14) 0.0322(14) 0.0043(12) -0.0034(11) 0.0011(12)
C9 0.0322(13) 0.0318(15) 0.0261(13) 0.0006(12) 0.0033(10) -0.0044(11)
C10 0.0264(12) 0.0278(15) 0.0349(14) -0.0050(12) 0.0011(10) -0.0006(11)
C11 0.0244(11) 0.0273(14) 0.0319(13) -0.0008(12) -0.0023(9) 0.0005(10)
C12 0.0280(12) 0.0290(15) 0.0305(13) 0.0031(12) 0.0006(10) 0.0026(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
O1 C5 1.234(4) . ?
N1 C4 1.453(4) . ?
N1 C5 1.347(4) . ?
N1 C12 1.447(3) . ?
C1 H1 0.9800 . ?
C1 C2 1.518(4) . ?
C1 C3 1.499(4) . ?
C1 C6 1.488(4) . ?
C2 H2 0.9800 . ?
C2 C3 1.498(4) . ?
C2 C5 1.491(4) . ?
C3 H3 0.9800 . ?
C3 C4 1.517(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C7 1.395(4) . ?
C6 C11 1.404(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.388(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.383(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.392(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.384(4) . ?
C11 H11 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
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
C5 N1 C4 114.7(2) . . ?
C5 N1 C12 124.0(2) . . ?
C12 N1 C4 121.2(2) . . ?
C2 C1 H1 115.7 . . ?
C3 C1 H1 115.7 . . ?
C3 C1 C2 59.5(2) . . ?
C6 C1 H1 115.7 . . ?
C6 C1 C2 118.8(2) . . ?
C6 C1 C3 119.7(2) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 59.60(19) . . ?
C3 C2 H2 120.0 . . ?
C5 C2 C1 115.2(2) . . ?
C5 C2 H2 120.0 . . ?
C5 C2 C3 106.7(2) . . ?
C1 C3 H3 119.3 . . ?
C1 C3 C4 117.0(2) . . ?
C2 C3 C1 60.87(18) . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 106.5(2) . . ?
C4 C3 H3 119.3 . . ?
N1 C4 C3 104.1(2) . . ?
N1 C4 H4A 110.9 . . ?
N1 C4 H4B 110.9 . . ?
C3 C4 H4A 110.9 . . ?
C3 C4 H4B 110.9 . . ?
H4A C4 H4B 109.0 . . ?
O1 C5 N1 125.5(3) . . ?
O1 C5 C2 126.6(3) . . ?
N1 C5 C2 107.9(2) . . ?
C7 C6 C1 119.7(2) . . ?
C7 C6 C11 118.0(2) . . ?
C11 C6 C1 122.2(2) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.7(3) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 121.0(3) . . ?
C9 C8 H8 119.5 . . ?
C8 C9 H9 120.6 . . ?
C8 C9 C10 118.9(3) . . ?
C10 C9 H9 120.6 . . ?
C9 C10 H10 119.7 . . ?
C11 C10 C9 120.6(3) . . ?
C11 C10 H10 119.7 . . ?
C6 C11 H11 119.6 . . ?
C10 C11 C6 120.8(3) . . ?
C10 C11 H11 119.6 . . ?
N1 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
N1 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
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 C4 -112.1(3) . . . . ?
C1 C2 C5 O1 -115.8(3) . . . . ?
C1 C2 C5 N1 63.8(3) . . . . ?
C1 C3 C4 N1 -61.8(4) . . . . ?
C1 C6 C7 C8 178.4(3) . . . . ?
C1 C6 C11 C10 -177.6(3) . . . . ?
C2 C1 C3 C4 94.6(3) . . . . ?
C2 C1 C6 C7 -148.2(3) . . . . ?
C2 C1 C6 C11 31.3(4) . . . . ?
C2 C3 C4 N1 3.4(3) . . . . ?
C3 C1 C2 C5 -95.3(3) . . . . ?
C3 C1 C6 C7 142.5(3) . . . . ?
C3 C1 C6 C11 -38.1(4) . . . . ?
C3 C2 C5 O1 -179.5(3) . . . . ?
C3 C2 C5 N1 0.1(3) . . . . ?
C4 N1 C5 O1 -178.1(3) . . . . ?
C4 N1 C5 C2 2.3(3) . . . . ?
C5 N1 C4 C3 -3.7(3) . . . . ?
C5 C2 C3 C1 109.9(2) . . . . ?
C5 C2 C3 C4 -2.2(3) . . . . ?
C6 C1 C2 C3 -109.5(2) . . . . ?
C6 C1 C2 C5 155.2(2) . . . . ?
C6 C1 C3 C2 107.9(3) . . . . ?
C6 C1 C3 C4 -157.4(3) . . . . ?
C6 C7 C8 C9 -0.2(4) . . . . ?
C7 C6 C11 C10 1.8(4) . . . . ?
C7 C8 C9 C10 0.7(4) . . . . ?
C8 C9 C10 C11 0.0(4) . . . . ?
C9 C10 C11 C6 -1.3(4) . . . . ?
C11 C6 C7 C8 -1.1(4) . . . . ?
C12 N1 C4 C3 178.6(2) . . . . ?
C12 N1 C5 O1 -0.4(4) . . . . ?
C12 N1 C5 C2 -180.0(2) . . . . ?
_shelx_res_file
;
TITL fasac13_a.res in P2(1)
fasac13.res
created by SHELXL-2018/3 at 10:39:01 on 22-Aug-2019
REM Old TITL FASAC13 in P2(1)
REM SHELXT solution in P2(1): R1 0.101, Rweak 0.042, Alpha 0.002
REM 0.631 for 6 systematic absences, Orientation as input
REM Flack x = -0.133 ( 0.302 ) from 801 Parsons' quotients
REM Formula found by SHELXT: C12 N O
CELL 1.54184 5.6803 9.2798 9.3092 90 90.739 90
ZERR 2 0.0002 0.0003 0.0003 0 0.003 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O
UNIT 24 26 2 2
L.S. 12
PLAN 12
SIZE 0.145 0.066 0.035
BOND $H
list 4
CONF
fmap 2
acta 149.008
REM
REM
REM
WGHT 0.066400 0.039600
FVAR 1.63134
O1 4 0.934065 0.749862 0.590265 11.00000 0.06797 0.03053 =
0.03897 -0.00660 0.01012 -0.02119
N1 3 0.804743 0.583923 0.424226 11.00000 0.02840 0.02218 =
0.02678 -0.00073 0.00041 -0.00052
C1 1 0.583603 0.450146 0.671469 11.00000 0.02171 0.02213 =
0.03010 -0.00050 -0.00127 0.00090
AFIX 13
H1 2 0.735187 0.400837 0.662054 11.00000 -1.20000
AFIX 0
C2 1 0.579420 0.607227 0.625957 11.00000 0.03657 0.02271 =
0.03163 0.00307 0.00457 0.00617
AFIX 13
H2 2 0.481740 0.676503 0.677738 11.00000 -1.20000
AFIX 0
C3 1 0.465777 0.494290 0.533341 11.00000 0.02220 0.04428 =
0.03015 0.00112 -0.00046 -0.00248
AFIX 13
H3 2 0.293672 0.490696 0.525425 11.00000 -1.20000
AFIX 0
C4 1 0.611232 0.484565 0.398183 11.00000 0.02825 0.04749 =
0.02753 -0.00235 -0.00212 -0.01102
AFIX 23
H4A 2 0.668884 0.387288 0.383911 11.00000 -1.20000
H4B 2 0.519402 0.513319 0.314416 11.00000 -1.20000
AFIX 0
C5 1 0.792352 0.657692 0.548567 11.00000 0.04022 0.02012 =
0.02832 0.00120 0.00140 -0.00069
C6 1 0.438253 0.404693 0.795296 11.00000 0.02424 0.02141 =
0.02652 -0.00225 -0.00446 -0.00193
C7 1 0.515374 0.292445 0.883742 11.00000 0.02595 0.02477 =
0.03206 0.00054 -0.00124 0.00119
AFIX 43
H7 2 0.655329 0.245130 0.863302 11.00000 -1.20000
AFIX 0
C8 1 0.385466 0.250589 1.001958 11.00000 0.03658 0.02669 =
0.03220 0.00433 -0.00341 0.00109
AFIX 43
H8 2 0.439380 0.175311 1.059543 11.00000 -1.20000
AFIX 0
C9 1 0.177103 0.319174 1.035346 11.00000 0.03216 0.03176 =
0.02612 0.00065 0.00334 -0.00445
AFIX 43
H9 2 0.091777 0.291364 1.115306 11.00000 -1.20000
AFIX 0
C10 1 0.097281 0.430533 0.947233 11.00000 0.02637 0.02781 =
0.03489 -0.00501 0.00113 -0.00063
AFIX 43
H10 2 -0.042556 0.477562 0.968561 11.00000 -1.20000
AFIX 0
C11 1 0.224090 0.471961 0.828122 11.00000 0.02441 0.02729 =
0.03193 -0.00078 -0.00227 0.00051
AFIX 43
H11 2 0.166773 0.545210 0.769142 11.00000 -1.20000
AFIX 0
C12 1 0.988566 0.603407 0.319865 11.00000 0.02802 0.02899 =
0.03054 0.00309 0.00063 0.00264
AFIX 137
H12A 2 1.056021 0.511572 0.296729 11.00000 -1.50000
H12B 2 1.108495 0.665294 0.359208 11.00000 -1.50000
H12C 2 0.923161 0.646285 0.234409 11.00000 -1.50000
AFIX 0
HKLF 4
REM fasac13_a.res in P2(1)
REM wR2 = 0.1183, GooF = S = 1.057, Restrained GooF = 1.056 for all data
REM R1 = 0.0438 for 1854 Fo > 4sig(Fo) and 0.0482 for all 2033 data
REM 128 parameters refined using 1 restraints
END
WGHT 0.0657 0.0410
REM Highest difference peak 0.156, deepest hole -0.220, 1-sigma level 0.042
Q1 1 0.5086 0.4963 0.4532 11.00000 0.05 0.16
Q2 1 0.3300 0.4453 0.8157 11.00000 0.05 0.16
Q3 1 0.8635 0.7574 0.6801 11.00000 0.05 0.16
Q4 1 0.7478 0.1461 1.0088 11.00000 0.05 0.15
Q5 1 0.1851 0.4605 0.8993 11.00000 0.05 0.13
Q6 1 0.4155 0.1068 0.9906 11.00000 0.05 0.13
Q7 1 0.2392 0.4882 0.7010 11.00000 0.05 0.13
Q8 1 0.4791 0.2972 0.9704 11.00000 0.05 0.12
Q9 1 1.1854 0.6483 0.4062 11.00000 0.05 0.12
Q10 1 0.8646 0.1454 0.9614 11.00000 0.05 0.12
Q11 1 0.5338 0.4471 0.7534 11.00000 0.05 0.12
Q12 1 0.8756 0.5967 0.3596 11.00000 0.05 0.12
;
_shelx_res_checksum 81384
_shelx_hkl_file
;
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5 6 4 7.01 3.03
5 6 5 12.99 3.39
5 7 -4 11.69 2.50
5 7 -4 14.64 2.35
5 7 -3 57.16 5.33
5 7 -3 76.01 6.17
5 7 -2 44.72 5.75
5 7 -1 0.79 2.43
5 7 -1 1.64 2.42
5 7 -1 1.18 1.58
5 7 0 45.11 5.88
5 7 0 37.35 3.98
5 7 1 18.43 4.28
5 7 2 10.26 3.06
5 7 3 19.61 2.84
5 7 3 28.76 4.15
5 7 3 23.67 3.60
5 7 4 2.74 1.62
5 8 -2 7.39 1.62
5 8 -2 20.38 2.71
5 8 -1 8.30 1.92
5 8 -1 18.24 2.79
5 8 0 89.40 7.89
5 8 1 26.59 3.44
5 8 1 42.39 4.47
5 8 2 8.85 2.06
6 -6 -2 1.98 1.92
-6 -6 1 6.01 2.05
-6 -6 0 17.82 2.66
-6 -6 -1 28.78 3.82
6 -5 -3 12.20 3.13
6 -5 -2 57.16 6.57
6 -5 -1 180.67 14.16
-6 -5 0 15.51 3.26
6 -5 0 18.91 4.43
-6 -5 -1 35.05 4.27
6 -5 1 45.24 6.01
-6 -5 -2 1.76 1.77
6 -5 2 2.53 2.72
6 -4 -3 5.44 3.14
6 -4 -2 26.04 4.93
6 -4 -1 3.62 3.42
6 -4 0 178.33 14.96
6 -4 1 75.57 8.65
-6 -4 -2 17.55 3.37
-6 -4 -3 59.64 5.61
-6 -4 -4 4.48 1.94
-6 -4 -5 8.33 1.96
6 -3 -3 6.52 3.30
6 -3 -2 114.26 11.21
6 -3 -2 145.84 11.39
6 -3 -1 78.69 9.03
6 -3 -1 89.29 8.55
6 -3 0 25.24 5.28
6 -3 0 21.83 4.15
6 -3 1 11.26 3.05
-6 -3 -2 16.39 3.30
6 -3 2 17.76 3.24
-6 -3 -2 25.44 5.18
-6 -3 -3 6.27 3.82
-6 -3 -4 3.53 2.22
-6 -3 -5 8.60 2.42
6 -2 -5 19.50 2.97
6 -2 -4 56.06 5.85
6 -2 -3 18.18 3.70
6 -2 -3 15.89 3.13
6 -2 -2 48.55 5.86
6 -2 -2 51.15 6.39
6 -2 -2 56.41 6.20
6 -2 -2 48.83 6.35
6 -2 -1 81.12 8.24
6 -2 -1 66.54 8.19
6 -2 -1 93.72 8.93
6 -2 0 89.52 8.47
6 -2 0 86.87 8.42
6 -2 0 75.77 8.92
6 -2 0 87.65 9.03
6 -2 1 5.74 2.96
6 -2 1 3.03 2.10
6 -2 1 4.96 2.81
-6 -2 -1 -1.66 3.81
6 -2 2 25.16 4.26
6 -2 2 19.52 3.80
6 -2 2 26.62 4.23
-6 -2 -2 26.51 5.89
-6 -2 -3 1.46 3.08
6 -2 3 -0.57 1.73
6 -2 3 3.28 2.25
-6 -2 -3 -1.20 4.08
-6 -2 -4 1.40 2.69
-6 -2 -4 6.88 2.41
6 -2 4 8.58 2.22
-6 -2 -4 4.85 3.57
-6 -2 -5 3.81 2.46
6 -1 -6 21.14 2.75
6 -1 -5 12.59 2.74
6 -1 -4 45.98 5.79
6 -1 -4 51.92 5.88
6 -1 -4 50.98 5.36
6 -1 -3 23.67 3.77
6 -1 -3 22.35 4.43
6 -1 -3 25.63 4.10
6 -1 -3 21.29 4.24
6 -1 -2 22.80 4.19
6 -1 -2 25.50 4.80
6 -1 -2 23.43 4.20
6 -1 -1 4.81 3.08
6 -1 -1 3.45 2.85
6 -1 -1 2.37 3.00
6 -1 0 168.87 13.62
6 -1 0 172.39 13.85
6 -1 0 172.58 14.50
6 -1 1 337.22 22.66
6 -1 1 345.73 22.63
6 -1 1 326.07 23.46
-6 -1 -1 287.47 24.64
6 -1 2 115.10 10.23
6 -1 2 126.61 9.94
6 -1 2 143.61 11.33
6 -1 2 107.74 10.76
-6 -1 -2 120.82 13.25
-6 -1 -3 -0.57 3.19
6 -1 3 2.23 2.04
6 -1 3 1.44 2.02
6 -1 3 1.86 2.32
-6 -1 -3 7.51 4.86
-6 -1 -4 5.97 3.92
-6 -1 -4 8.54 3.18
6 -1 4 5.17 2.13
6 -1 4 4.21 2.28
-6 -1 -4 11.17 4.49
-6 -1 -5 31.83 4.16
6 0 -6 2.46 1.57
6 0 -5 2.07 2.05
6 0 -5 0.22 1.33
6 0 -4 8.04 2.93
6 0 -4 8.51 2.61
6 0 -4 8.80 2.58
6 0 -3 14.89 3.26
6 0 -3 15.46 4.11
6 0 -3 16.96 3.61
6 0 -3 20.32 3.90
6 0 -2 24.71 4.23
6 0 -2 19.60 4.21
6 0 -2 17.58 4.21
6 0 -2 23.36 4.52
6 0 -1 -0.46 2.71
6 0 0 27.88 4.98
6 0 0 35.50 5.35
6 0 0 44.09 5.94
6 0 0 35.61 5.77
6 0 1 15.00 3.96
6 0 1 17.27 3.79
6 0 1 12.96 3.60
-6 0 -2 4.15 3.74
6 0 2 2.09 2.37
6 0 2 2.63 1.96
6 0 2 7.38 2.99
6 0 2 2.33 3.51
-6 0 -3 3.72 3.61
-6 0 -3 -0.54 3.54
6 0 3 1.70 1.92
6 0 3 4.61 2.47
6 0 3 4.55 3.47
-6 0 -3 -1.46 5.01
-6 0 -4 1.17 3.76
-6 0 -4 3.10 3.21
-6 0 -4 -0.28 2.14
6 0 4 3.71 2.07
-6 0 -4 3.94 4.33
6 0 5 217.35 13.75
6 0 5 166.03 12.40
-6 0 -5 197.12 16.31
-6 0 -6 5.88 2.08
6 1 -6 17.54 2.56
6 1 -6 10.09 1.74
6 1 -5 12.56 2.71
6 1 -5 8.79 1.99
6 1 -5 9.63 2.37
6 1 -4 52.15 6.01
6 1 -4 45.69 5.53
6 1 -4 59.00 5.99
6 1 -3 22.88 3.72
6 1 -3 28.64 4.74
6 1 -3 25.46 4.41
6 1 -3 27.24 4.21
6 1 -3 23.65 3.94
6 1 -2 24.48 4.22
6 1 -2 31.10 4.90
6 1 -2 24.27 4.54
6 1 -2 24.82 4.27
6 1 -2 17.99 4.00
6 1 -1 1.40 2.61
6 1 -1 1.31 2.59
6 1 -1 1.09 1.95
6 1 -1 6.46 3.00
6 1 0 186.09 14.10
6 1 0 166.44 14.24
6 1 0 165.42 13.92
6 1 1 325.34 23.09
6 1 1 329.75 23.41
6 1 1 349.69 23.85
6 1 1 360.77 25.90
6 1 2 123.24 10.56
6 1 2 114.72 10.42
6 1 2 142.17 11.36
6 1 2 151.51 13.46
-6 1 -3 5.18 3.75
6 1 3 3.02 2.10
6 1 3 5.09 2.50
6 1 3 3.15 3.52
-6 1 -4 6.50 3.93
6 1 4 9.56 2.69
6 1 4 8.01 3.31
-6 1 -4 9.19 4.86
6 1 5 26.38 3.96
6 2 -6 29.59 3.00
6 2 -5 19.92 3.14
6 2 -5 20.28 3.11
6 2 -4 50.36 5.52
6 2 -4 52.85 5.44
6 2 -3 15.89 3.04
6 2 -3 14.95 3.29
6 2 -3 16.92 3.56
6 2 -3 16.10 3.42
6 2 -3 12.38 2.76
6 2 -2 53.65 5.96
6 2 -2 49.15 6.02
6 2 -2 42.49 5.62
6 2 -2 45.25 5.85
6 2 -1 79.54 8.52
6 2 -1 79.93 8.12
6 2 -1 72.45 7.31
6 2 -1 64.63 7.64
6 2 0 89.69 8.55
6 2 0 81.57 8.93
6 2 0 83.34 8.66
6 2 0 75.95 7.49
6 2 0 103.13 10.65
6 2 1 2.58 2.50
6 2 1 5.40 2.62
6 2 1 0.40 2.29
6 2 2 18.19 3.75
6 2 2 21.91 3.86
6 2 2 27.23 4.12
6 2 2 17.76 5.33
6 2 3 2.54 1.79
6 2 3 2.15 1.58
6 2 3 3.12 2.17
6 2 3 -3.07 3.69
-6 2 -4 11.58 4.11
6 2 4 7.22 2.32
6 2 4 6.67 3.20
6 2 5 2.84 2.17
6 3 -5 45.84 4.40
6 3 -4 4.03 1.82
6 3 -4 7.56 2.30
6 3 -4 5.90 2.17
6 3 -3 8.13 2.27
6 3 -3 2.87 2.16
6 3 -3 6.26 2.55
6 3 -3 6.33 2.43
6 3 -2 149.27 11.13
6 3 -2 143.40 11.39
6 3 -2 145.23 11.08
6 3 -2 115.64 10.29
6 3 -1 92.37 8.19
6 3 -1 75.68 7.28
6 3 -1 69.40 7.54
6 3 0 19.95 3.82
6 3 0 22.88 4.11
6 3 0 17.22 3.16
6 3 0 23.19 5.02
6 3 1 9.56 2.94
6 3 1 9.09 3.04
6 3 1 17.39 4.60
6 3 2 21.27 3.70
6 3 3 15.74 2.78
6 3 3 10.19 2.32
6 3 3 12.55 4.36
6 3 4 0.76 2.66
6 3 5 6.35 2.24
6 4 -5 23.33 2.54
6 4 -5 21.77 2.57
6 4 -4 7.29 1.93
6 4 -4 6.75 1.99
6 4 -3 4.91 1.71
6 4 -3 5.07 2.06
6 4 -3 6.26 2.21
6 4 -3 9.24 2.24
6 4 -2 36.41 4.32
6 4 -2 28.43 4.39
6 4 -2 30.42 4.18
6 4 -2 28.72 4.00
6 4 -1 2.04 1.88
6 4 -1 2.28 1.76
6 4 -1 3.06 1.84
6 4 0 178.06 13.48
6 4 0 197.48 13.25
6 4 0 170.15 12.31
6 4 1 75.63 7.00
6 4 1 63.94 7.67
6 4 2 19.17 3.25
6 4 2 28.76 4.75
6 4 3 58.74 4.88
6 4 3 47.08 4.78
6 4 4 7.83 2.66
6 5 -4 18.31 2.24
6 5 -3 9.87 1.74
6 5 -3 11.96 2.06
6 5 -3 16.36 2.25
6 5 -3 18.07 2.50
6 5 -2 73.30 5.86
6 5 -2 59.13 5.86
6 5 -2 59.41 5.27
6 5 -2 59.53 5.44
6 5 -1 163.58 10.94
6 5 -1 159.73 11.09
6 5 0 18.38 3.24
6 5 1 43.06 4.70
6 5 1 43.43 4.96
6 5 2 1.13 1.33
6 5 2 -1.11 2.03
6 5 3 17.84 3.31
6 6 -1 7.76 1.83
6 6 -1 11.45 2.08
6 6 0 22.70 2.84
6 6 1 80.18 6.18
7 -1 -1 15.12 2.47
7 -1 0 5.06 1.78
7 -1 1 41.75 4.05
7 0 -2 -0.17 1.04
7 0 -1 5.16 1.58
7 0 0 1.02 1.37
7 0 0 2.63 1.24
7 0 0 0.81 1.42
7 0 1 3.20 1.53
7 0 2 121.77 8.46
7 1 -2 23.94 2.69
7 1 -2 30.50 3.21
7 1 -1 16.63 2.44
7 1 -1 17.41 2.56
7 1 0 3.90 1.54
7 1 0 3.94 1.50
7 1 1 48.95 4.07
7 1 1 35.95 4.07
7 1 2 24.09 2.80
7 2 -1 7.49 1.56
7 2 -1 4.41 1.44
7 2 0 6.14 1.48
7 2 0 5.02 1.37
7 2 0 6.15 1.60
7 2 1 11.69 1.79
0 0 0 0.00 0.00
TITL FASAC13 in P2(1)
REM P2(1) (#4 in standard setting)
CELL 1.54184 5.680289 9.279777 9.309164 90.0000 90.7387 90.0000
ZERR 2.00 0.000156 0.000303 0.000303 0.0000 0.0028 0.0000
LATT -1
SYMM -x, y+1/2,-z
SFAC C H N O
UNIT 22.00 28.00 2.00 2.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 82585
_olex2_submission_original_sample_id fasac13
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.041
_oxdiff_exptl_absorpt_empirical_full_min 0.541