#######################################################################
#
# 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_p167
_audit_block_doi 10.5517/ccdc.csd.cc27j6cc
_database_code_depnum_ccdc_archive 'CCDC 2071152'
loop_
_audit_author_name
_audit_author_address
'Vincent Lynch'
;University of Texas at Austin
United States of America
;
_audit_update_record
;
2021-03-17 deposited with the CCDC. 2021-08-05 downloaded from the CCDC.
;
_audit_creation_date 2021-02-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C9 H14 O3'
_chemical_formula_sum 'C9 H14 O3'
_chemical_formula_weight 170.20
_chemical_absolute_configuration ad
_chemical_melting_point ?
_chemical_oxdiff_formula C9H14O3
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'
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 orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_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'
_cell_length_a 7.60780(15)
_cell_length_b 9.1979(2)
_cell_length_c 13.39653(18)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 937.43(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 6284
_cell_measurement_temperature 100.02(10)
_cell_measurement_theta_max 73.1310
_cell_measurement_theta_min 5.8170
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.738
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.269
_exptl_absorpt_correction_type 'gaussian and multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.70a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.206
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 368
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.2795
0 0 1 0.2795
1 1 0 0.0439
-1 -1 0 0.0669
-3 4 -1 0.0880
3 -4 1 0.0300
3 5 0 0.0589
-3 -5 0 0.0699
_exptl_crystal_size_max 0.574
_exptl_crystal_size_mid 0.118
_exptl_crystal_size_min 0.111
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0008 0.0012 -0.9999 -0.0197 0.1132 0.0034
0.0008 -0.0012 0.9999 0.0197 -0.1132 -0.0034
1.0012 0.9962 0.0026 0.0788 0.0060 0.2503
-1.0012 -0.9962 -0.0026 -0.0788 -0.0060 -0.2503
-3.4021 4.2895 -0.8209 -0.9705 -0.0771 0.2286
3.4021 -4.2895 0.8209 0.9705 0.0771 -0.2286
3.0085 4.9865 0.0160 0.0587 -0.0213 1.0318
-3.0085 -4.9865 -0.0160 -0.0587 0.0213 -1.0318
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0235
_diffrn_reflns_av_unetI/netI 0.0138
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 8913
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 73.267
_diffrn_reflns_theta_min 5.835
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.02(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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 -129.00 47.00 1.00 4.00 -- -41.34 0.00-120.00 176
2 \w 27.00 97.00 1.00 4.00 -- 41.34-125.00-180.00 70
3 \w 97.00 178.00 1.00 13.00 -- 107.09 125.00 60.00 81
4 \w 34.00 133.00 1.00 13.00 -- 107.09 -45.00 150.00 99
5 \w 103.00 178.00 1.00 13.00 -- 107.09 77.00 90.00 75
6 \w 97.00 178.00 1.00 13.00 -- 107.09 125.00 -60.00 81
7 \w 103.00 178.00 1.00 13.00 -- 107.09 77.00 150.00 75
8 \w 103.00 178.00 1.00 13.00 -- 107.09 77.00-180.00 75
9 \w 24.00 107.00 1.00 13.00 -- 107.09 -94.00 90.00 83
10 \w -113.00 -13.00 1.00 4.00 -- -41.34 -57.00 150.00 100
11 \w -113.00 -13.00 1.00 4.00 -- -41.34 -57.00 60.00 100
12 \w 81.00 178.00 1.00 13.00 -- 107.09 45.00 -90.00 97
13 \w 54.00 178.00 1.00 13.00 -- 107.09 15.00 150.00 124
14 \w 78.00 178.00 1.00 13.00 -- 107.09 61.00 -60.00 100
15 \w 79.00 178.00 1.00 13.00 -- 107.09 30.00 30.00 99
16 \w -113.00 -13.00 1.00 4.00 -- -41.34 -57.00-120.00 100
17 \w -87.00 -6.00 1.00 4.00 -- -41.34 125.00 -90.00 81
18 \w 78.00 109.00 1.00 13.00 -- 107.09 61.00-150.00 31
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.1677343000
_diffrn_orient_matrix_UB_12 -0.0894838000
_diffrn_orient_matrix_UB_13 0.0194619000
_diffrn_orient_matrix_UB_21 0.0255875000
_diffrn_orient_matrix_UB_22 -0.0193517000
_diffrn_orient_matrix_UB_23 -0.1132875000
_diffrn_orient_matrix_UB_31 0.1104783000
_diffrn_orient_matrix_UB_32 0.1402848000
_diffrn_orient_matrix_UB_33 -0.0032849000
_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 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.681
_reflns_Friedel_fraction_full 1.000
_reflns_Friedel_fraction_max 0.973
_reflns_number_gt 1831
_reflns_number_total 1862
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_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 1.171.41.70a (Rigaku OD, 2020)'
_computing_data_collection 'CrysAlisPro 1.171.41.70a (Rigaku OD, 2020)'
_computing_data_reduction 'CrysAlisPro 1.171.41.70a (Rigaku OD, 2020)'
_computing_molecular_graphics 'Shelxtl-Plus/XP, Bruker AXS, Inc. 2009'
_computing_publication_material 'Shlelxtl-Plus, Bruker AXS, Inc. 2009'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max 0.214
_refine_diff_density_min -0.207
_refine_diff_density_rms 0.038
_refine_ls_abs_structure_details
;
Flack x determined using 735 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.06(6)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.127
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 116
_refine_ls_number_reflns 1862
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0281
_refine_ls_R_factor_gt 0.0277
_refine_ls_restrained_S_all 1.127
_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^)+(0.0416P)^2^+0.1297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0732
_refine_ls_wR_factor_ref 0.0738
_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:
C4(H4), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
C8(H8A,H8B)
2.c Idealised Me refined as rotating group:
C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_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
O1 O 0.28350(14) 0.61962(11) 0.46678(7) 0.0198(2) Uani 1 1 d . . . . .
O2 O 0.25401(15) 0.40629(11) 0.53765(7) 0.0235(3) Uani 1 1 d . . . . .
O3 O 0.16168(16) 0.43639(12) 0.19449(8) 0.0258(3) Uani 1 1 d . . . . .
H3 H 0.191(4) 0.495(3) 0.143(2) 0.057(7) Uiso 1 1 d . . . . .
C1 C 0.2392(2) 0.47883(16) 0.46070(10) 0.0188(3) Uani 1 1 d . . . . .
C2 C 0.18304(19) 0.41658(16) 0.36672(11) 0.0194(3) Uani 1 1 d . . . . .
C3 C 0.20004(19) 0.49668(16) 0.28250(10) 0.0191(3) Uani 1 1 d . . . . .
C4 C 0.2707(2) 0.64989(16) 0.28458(10) 0.0192(3) Uani 1 1 d . . . . .
H4 H 0.206107 0.707148 0.232823 0.023 Uiso 1 1 calc R U . . .
C5 C 0.2281(2) 0.71612(15) 0.38621(10) 0.0184(3) Uani 1 1 d . . . . .
H5 H 0.097902 0.729301 0.390825 0.022 Uiso 1 1 calc R U . . .
C6 C 0.1270(2) 0.26014(17) 0.36768(11) 0.0242(3) Uani 1 1 d . . . . .
H6A H 0.218124 0.201168 0.399824 0.036 Uiso 1 1 calc R U . . .
H6B H 0.109567 0.226469 0.298987 0.036 Uiso 1 1 calc R U . . .
H6C H 0.016644 0.250629 0.404867 0.036 Uiso 1 1 calc R U . . .
C7 C 0.4665(2) 0.65030(18) 0.25624(11) 0.0247(3) Uani 1 1 d . . . . .
H7A H 0.533524 0.596345 0.306533 0.037 Uiso 1 1 calc R U . . .
H7B H 0.509119 0.750740 0.253231 0.037 Uiso 1 1 calc R U . . .
H7C H 0.481582 0.604076 0.190895 0.037 Uiso 1 1 calc R U . . .
C8 C 0.3150(2) 0.86101(17) 0.40749(11) 0.0221(3) Uani 1 1 d . . . . .
H8A H 0.285564 0.929885 0.353222 0.026 Uiso 1 1 calc R U . . .
H8B H 0.444151 0.847829 0.407782 0.026 Uiso 1 1 calc R U . . .
C9 C 0.2581(2) 0.92644(17) 0.50725(11) 0.0249(3) Uani 1 1 d . . . . .
H9A H 0.131300 0.945244 0.505987 0.037 Uiso 1 1 calc R U . . .
H9B H 0.321180 1.017876 0.518475 0.037 Uiso 1 1 calc R U . . .
H9C H 0.285238 0.858164 0.561245 0.037 Uiso 1 1 calc R U . . .
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 0.0259(5) 0.0212(5) 0.0122(4) 0.0010(4) -0.0016(4) 0.0002(4)
O2 0.0334(6) 0.0235(5) 0.0137(5) 0.0031(4) -0.0005(4) 0.0012(5)
O3 0.0380(7) 0.0271(6) 0.0124(5) -0.0009(4) -0.0028(4) -0.0055(5)
C1 0.0188(7) 0.0225(7) 0.0149(6) 0.0010(5) 0.0012(5) 0.0014(6)
C2 0.0200(7) 0.0224(7) 0.0157(6) -0.0003(6) 0.0004(5) 0.0007(6)
C3 0.0191(6) 0.0245(7) 0.0136(6) -0.0010(6) -0.0005(5) 0.0009(6)
C4 0.0218(7) 0.0227(7) 0.0132(6) 0.0016(5) -0.0003(5) 0.0002(6)
C5 0.0210(7) 0.0200(7) 0.0142(6) 0.0027(5) 0.0002(5) 0.0012(6)
C6 0.0290(8) 0.0236(7) 0.0199(7) 0.0003(6) 0.0002(6) -0.0041(6)
C7 0.0242(8) 0.0309(8) 0.0190(7) -0.0031(6) 0.0051(6) -0.0027(7)
C8 0.0254(8) 0.0219(7) 0.0188(7) -0.0005(6) 0.0017(6) -0.0011(6)
C9 0.0284(8) 0.0240(7) 0.0225(7) -0.0034(6) 0.0002(6) -0.0001(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
O1 C1 1.3405(18) . ?
O1 C5 1.4596(16) . ?
O2 C1 1.2331(18) . ?
O3 H3 0.90(3) . ?
O3 C3 1.3353(17) . ?
C1 C2 1.4476(19) . ?
C2 C3 1.354(2) . ?
C2 C6 1.501(2) . ?
C3 C4 1.509(2) . ?
C4 H4 1.0000 . ?
C4 C5 1.5263(18) . ?
C4 C7 1.537(2) . ?
C5 H5 1.0000 . ?
C5 C8 1.515(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.5283(19) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
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 C5 118.03(11) . . ?
C3 O3 H3 112.0(17) . . ?
O1 C1 C2 120.61(12) . . ?
O2 C1 O1 116.67(13) . . ?
O2 C1 C2 122.68(13) . . ?
C1 C2 C6 117.11(13) . . ?
C3 C2 C1 118.77(13) . . ?
C3 C2 C6 123.79(13) . . ?
O3 C3 C2 119.28(13) . . ?
O3 C3 C4 118.82(12) . . ?
C2 C3 C4 121.81(13) . . ?
C3 C4 H4 107.7 . . ?
C3 C4 C5 108.27(11) . . ?
C3 C4 C7 110.07(12) . . ?
C5 C4 H4 107.7 . . ?
C5 C4 C7 115.16(12) . . ?
C7 C4 H4 107.7 . . ?
O1 C5 C4 110.83(11) . . ?
O1 C5 H5 108.3 . . ?
O1 C5 C8 105.66(11) . . ?
C4 C5 H5 108.3 . . ?
C8 C5 C4 115.24(12) . . ?
C8 C5 H5 108.3 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.0 . . ?
C5 C8 H8B 109.0 . . ?
C5 C8 C9 112.80(13) . . ?
H8A C8 H8B 107.8 . . ?
C9 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
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
_geom_hbond_publ_flag
O3 H3 O2 0.90(3) 1.73(3) 2.6305(15) 175(3) 2_564 yes
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
O1 C1 C2 C3 9.4(2) . . . . ?
O1 C1 C2 C6 -176.92(13) . . . . ?
O1 C5 C8 C9 -61.03(15) . . . . ?
O2 C1 C2 C3 -168.37(14) . . . . ?
O2 C1 C2 C6 5.3(2) . . . . ?
O3 C3 C4 C5 155.29(13) . . . . ?
O3 C3 C4 C7 -78.02(16) . . . . ?
C1 O1 C5 C4 -47.87(16) . . . . ?
C1 O1 C5 C8 -173.35(12) . . . . ?
C1 C2 C3 O3 174.77(13) . . . . ?
C1 C2 C3 C4 -1.8(2) . . . . ?
C2 C3 C4 C5 -28.11(18) . . . . ?
C2 C3 C4 C7 98.57(16) . . . . ?
C3 C4 C5 O1 50.63(15) . . . . ?
C3 C4 C5 C8 170.53(12) . . . . ?
C4 C5 C8 C9 176.26(13) . . . . ?
C5 O1 C1 O2 -165.22(12) . . . . ?
C5 O1 C1 C2 16.85(19) . . . . ?
C6 C2 C3 O3 1.6(2) . . . . ?
C6 C2 C3 C4 -175.00(13) . . . . ?
C7 C4 C5 O1 -73.04(15) . . . . ?
C7 C4 C5 C8 46.86(17) . . . . ?
_shelx_res_file
;
TITL p167_a.res in P2(1)2(1)2(1)
p167.res
created by SHELXL-2018/3 at 16:19:21 on 09-Feb-2021
REM Old TITL P167 in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.100, Rweak 0.023, Alpha 0.003, Orientation as input
REM Flack x = 0.329 ( 0.154 ) from Parsons' quotients
REM Formula found by SHELXT: C9 O3
rem ISOR 0.01 0.02
CELL 1.54184 7.607796 9.197913 13.39653 90 90 90
ZERR 4 0.00015 0.000196 0.000177 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 O
UNIT 36 56 12
EQIV $1 0.5-X,1-Y,-0.5+Z
L.S. 8 0 0
PLAN 2
TEMP -173
CONF
HTAB O3 O2_$1
BOND $H
list 4
MORE -1
fmap 2 53
acta
REM
REM
REM
WGHT 0.041600 0.129700
FVAR 6.86634
O1 3 0.283505 0.619620 0.466782 11.00000 0.02593 0.02117 =
0.01217 0.00098 -0.00156 0.00024
O2 3 0.254014 0.406294 0.537652 11.00000 0.03340 0.02347 =
0.01374 0.00313 -0.00050 0.00119
O3 3 0.161676 0.436391 0.194485 11.00000 0.03796 0.02710 =
0.01238 -0.00094 -0.00284 -0.00550
H3 2 0.191008 0.494621 0.142993 11.00000 0.05718
C1 1 0.239217 0.478835 0.460699 11.00000 0.01884 0.02252 =
0.01493 0.00100 0.00117 0.00143
C2 1 0.183040 0.416576 0.366723 11.00000 0.02002 0.02240 =
0.01571 -0.00031 0.00037 0.00072
C3 1 0.200042 0.496675 0.282504 11.00000 0.01909 0.02450 =
0.01360 -0.00102 -0.00053 0.00090
C4 1 0.270740 0.649889 0.284584 11.00000 0.02176 0.02271 =
0.01323 0.00159 -0.00033 0.00018
AFIX 13
H4 2 0.206107 0.707148 0.232823 11.00000 -1.20000
AFIX 0
C5 1 0.228123 0.716118 0.386210 11.00000 0.02097 0.02000 =
0.01420 0.00273 0.00019 0.00118
AFIX 13
H5 2 0.097902 0.729301 0.390825 11.00000 -1.20000
AFIX 0
C6 1 0.126980 0.260139 0.367684 11.00000 0.02898 0.02363 =
0.01987 0.00030 0.00022 -0.00409
AFIX 137
H6A 2 0.218124 0.201168 0.399824 11.00000 -1.50000
H6B 2 0.109567 0.226469 0.298987 11.00000 -1.50000
H6C 2 0.016644 0.250629 0.404867 11.00000 -1.50000
AFIX 0
C7 1 0.466467 0.650300 0.256244 11.00000 0.02423 0.03090 =
0.01897 -0.00306 0.00505 -0.00273
AFIX 137
H7A 2 0.533524 0.596345 0.306533 11.00000 -1.50000
H7B 2 0.509119 0.750740 0.253231 11.00000 -1.50000
H7C 2 0.481582 0.604076 0.190895 11.00000 -1.50000
AFIX 0
C8 1 0.315002 0.861009 0.407493 11.00000 0.02540 0.02194 =
0.01884 -0.00048 0.00171 -0.00110
AFIX 23
H8A 2 0.285564 0.929885 0.353222 11.00000 -1.20000
H8B 2 0.444151 0.847829 0.407782 11.00000 -1.20000
AFIX 0
C9 1 0.258074 0.926442 0.507247 11.00000 0.02844 0.02395 =
0.02245 -0.00338 0.00024 -0.00008
AFIX 137
H9A 2 0.131300 0.945244 0.505987 11.00000 -1.50000
H9B 2 0.321180 1.017876 0.518475 11.00000 -1.50000
H9C 2 0.285238 0.858164 0.561245 11.00000 -1.50000
AFIX 0
HKLF 4
REM p167_a.res in P2(1)2(1)2(1)
REM wR2 = 0.0738, GooF = S = 1.127, Restrained GooF = 1.127 for all data
REM R1 = 0.0277 for 1831 Fo > 4sig(Fo) and 0.0281 for all 1862 data
REM 116 parameters refined using 0 restraints
END
WGHT 0.0416 0.1297
REM Highest difference peak 0.214, deepest hole -0.207, 1-sigma level 0.038
Q1 1 0.2354 0.5733 0.2836 11.00000 0.05 0.21
Q2 1 0.3660 0.6460 0.2753 11.00000 0.05 0.19
;
_shelx_res_checksum 99009
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-8 2 1 3531.05 139.361 15
8 2 -1 3240.41 143.866 7
8 -2 1 3485.07 150.374 7
-8 2 0 988.841 72.0722 15
8 2 0 847.909 72.3988 7
8 -2 0 1014.21 82.7475 7
8 -2 -1 3174.28 129.119 8
-8 2 -1 3402.61 134.204 15
8 2 1 3206.50 136.887 7
8 -2 -1 3374.78 148.542 7
8 -2 -2 5695.31 184.573 8
-8 2 -2 6393.03 185.674 15
8 2 2 5826.45 179.158 7
8 -2 -2 6237.64 202.166 7
8 -2 -3 1798.15 99.5716 8
-8 2 -3 1892.59 93.9051 15
8 -2 -3 1937.48 106.364 7
8 -2 -4 3091.38 129.897 8
-8 2 -4 3423.14 123.042 15
8 -2 -4 3244.46 131.831 7
8 -2 -5 2650.63 116.554 8
-8 2 -5 2981.94 108.467 15
8 -2 -5 2791.20 113.612 7
8 -2 -6 7089.71 189.075 8
8 -2 -6 6796.13 172.298 7
8 -2 -7 1766.75 79.9960 8
-8 2 -7 1843.11 74.3531 15
8 -2 -8 1222.86 57.6877 8
-8 2 -8 1366.87 55.6750 15
8 -3 7 5467.61 126.426 13
-8 3 6 128.915 25.6362 15
8 -3 6 122.043 23.6328 7
8 -3 6 102.563 20.7070 13
-8 3 5 1082.68 68.5530 15
8 -3 5 993.314 62.9717 7
8 -3 5 1045.81 60.9249 13
-8 3 4 1102.72 71.9424 15
8 -3 4 973.358 68.1804 7
8 -3 4 934.875 61.8937 13
-8 3 3 1350.37 82.0419 15
8 -3 3 1285.66 82.8548 7
8 -3 3 1265.24 75.9395 13
-8 3 2 3890.77 145.646 15
8 -3 2 3604.90 136.998 13
8 -3 2 3992.19 152.405 7
-8 3 1 47.5282 24.8124 15
8 3 -1 53.9551 23.2517 7
8 -3 1 15.6885 22.1437 7
-8 3 0 935.694 70.2904 15
8 3 0 878.321 67.6658 7
8 -3 0 920.979 73.8008 7
-8 3 -1-10.4916 24.8878 15
8 -3 -1 16.1768 17.4392 8
8 -3 -1 11.7331 22.3682 7
8 -3 -2 3517.16 139.062 8
-8 3 -2 3968.32 140.969 15
8 -3 -2 3841.64 147.704 7
8 -3 -3 1185.14 78.9387 8
-8 3 -3 1329.72 77.6422 15
8 -3 -3 1290.10 80.0227 7
8 -3 -4 1001.72 70.7350 8
-8 3 -4 962.770 62.7095 15
8 -3 -4 938.861 64.4238 7
8 -3 -5 1000.92 67.1285 8
-8 3 -5 1071.30 62.0212 15
8 -3 -5 953.427 58.2045 7
-8 3 -6 115.552 22.3713 15
8 -3 -6 118.103 23.3480 8
8 -3 -7 5843.09 146.680 8
-8 3 -7 6117.52 138.841 15
-8 4 6 353.649 33.4932 15
8 -4 6 301.094 31.2689 13
-8 4 5 1402.70 72.2324 15
8 -4 5 1311.60 66.5404 7
8 -4 5 1260.09 66.3259 13
-8 4 4 6004.67 167.549 15
8 -4 4 5703.58 155.229 13
8 -4 4 5671.10 160.931 7
-8 4 3 133.967 29.8958 15
8 -4 3 161.878 31.1911 7
8 -4 3 122.490 25.9848 13
-8 4 2 1771.11 92.5553 15
8 -4 2 1716.90 88.7196 13
8 -4 2 1881.49 96.3712 7
-8 4 1 4392.37 150.488 15
8 -4 1 4407.65 152.195 7
-8 4 0 1349.28 80.9965 15
8 -4 0 1300.58 81.1580 7
-8 4 -1 4355.15 145.614 15
8 -4 -1 4371.96 148.318 7
-8 4 -2 1852.22 89.8325 15
8 -4 -2 1560.60 86.0270 8
8 -4 -2 1628.13 86.0840 7
-8 4 -3 93.3930 24.1093 15
8 -4 -3 102.641 24.9659 8
8 -4 -3 144.880 26.5415 7
8 -4 -4 5239.92 157.960 8
-8 4 -4 5541.16 150.627 15
8 -4 -4 5389.58 142.493 7
8 -4 -5 1229.63 68.5499 8
-8 4 -5 1358.95 65.4146 15
8 -4 -6 331.100 32.7028 8
-8 4 -6 349.840 29.8624 15
-8 4 -6 368.524 34.0861 6
-8 5 5 1050.34 53.2631 15
8 -5 5 886.509 49.2773 13
-8 5 4 1878.92 79.2201 15
8 -5 4 1863.65 76.4964 7
-8 5 3 557.754 46.9055 15
8 -5 3 603.263 46.7861 7
-8 5 2 1433.75 74.2776 15
8 -5 2 1481.37 76.1218 7
-8 5 1 2260.48 95.2922 15
8 -5 1 2201.40 93.9736 7
-8 5 0 970.593 62.4527 15
8 -5 0 859.964 51.7681 8
8 -5 0 1055.14 63.8002 7
-8 5 -1 2199.36 91.2504 15
8 -5 -1 2153.08 89.3322 7
-8 5 -1 2072.06 80.7651 6
-8 5 -2 1430.98 70.7871 15
8 -5 -2 1340.38 70.4144 8
8 -5 -2 1320.85 66.1495 7
-8 5 -2 1495.94 69.6785 6
-8 5 -3 594.222 44.0428 15
8 -5 -3 543.281 45.0694 8
-8 5 -3 640.112 45.3409 6
-8 5 -4 1838.74 70.0682 15
8 -5 -4 1724.83 74.9252 8
-8 5 -4 1841.43 74.6962 6
9 0 0-18.0239 19.3969 7
9 0 -1-1.07049 15.8898 7
9 0 1 46.3772 19.2765 7
9 0 -2 571.569 49.3944 7
9 0 2 504.789 40.9770 7
9 0 -3 1691.64 79.1092 7
9 0 -4 75.7412 19.3252 7
9 1 -3 919.992 57.7924 7
9 1 -2 296.585 36.2061 7
9 -1 2 285.864 32.4951 7
-9 1 1 338.615 32.7711 15
9 1 -1 335.819 37.1810 7
9 -1 1 319.269 36.4656 7
-9 1 0 181.159 25.0359 15
9 1 0 208.996 29.6411 7
9 -1 0 223.126 32.8691 7
-9 1 -1 335.689 34.6251 15
9 1 1 260.971 30.5215 7
9 -1 -1 336.131 38.5917 7
-9 1 -2 330.297 33.3949 15
9 -1 -2 286.627 35.5884 7
-9 1 -3 970.292 51.8085 15
9 -1 -3 985.586 58.7356 7
-9 1 -4 414.638 32.7860 15
9 -1 -4 380.499 34.9433 7
-9 2 2 1626.82 68.4700 15
9 -2 2 1685.02 75.2487 7
-9 2 1 879.388 52.1556 15
9 -2 1 951.663 59.1705 7
-9 2 0 38.0813 16.9368 15
9 -2 0 92.8833 21.7167 7
-9 2 -1 922.307 53.8169 15
9 -2 -1 911.374 58.4058 7
-9 2 -2 1667.03 71.3956 15
9 -2 -2 1646.84 76.2925 7
-9 2 -3 4705.78 122.225 15
9 -2 -3 4604.50 125.886 7
9 -3 2 2695.24 89.1457 7
-9 3 1 1479.11 64.8972 15
9 -3 1 1443.20 67.0967 7
-9 3 0 2703.27 91.0324 15
9 -3 0 2830.96 96.6019 7
-9 3 -1 1494.52 65.4063 15
9 -3 -1 1553.89 69.1477 7
-9 3 -2 2781.40 88.6901 15
9 -3 -2 2682.27 88.1623 7
0 0 0 0.00 0.00 0
TITL P167abs in P2(1)2(1)2(1)
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 1.54184 7.607796 9.197913 13.396530 90.0000 90.0000 90.0000
ZERR 4.00 0.000150 0.000196 0.000177 0.0000 0.0000 0.0000
LATT -1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H O
UNIT 36.00 56.00 12.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.1; aver:100.0
TEMP -173
SIZE 0.11 0.12 0.57
TREF
HKLF 4
END
;
_shelx_hkl_checksum 83975
_olex2_date_sample_data_collection 2021-02-09
_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 1.772
_oxdiff_exptl_absorpt_empirical_full_min 0.684
#######################################################################
#
# 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_p127
_audit_block_doi 10.5517/ccdc.csd.cc27j6dd
_database_code_depnum_ccdc_archive 'CCDC 2071153'
loop_
_audit_author_name
_audit_author_address
'Vincent Lynch'
;University of Texas at Austin
United States of America
;
_audit_update_record
;
2021-03-17 deposited with the CCDC. 2021-08-05 downloaded from the CCDC.
;
_audit_creation_date 2021-03-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C9 H14 O3'
_chemical_formula_sum 'C9 H14 O3'
_chemical_formula_weight 170.20
_chemical_absolute_configuration ad
_chemical_melting_point ?
_chemical_oxdiff_formula C9H14O3
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'
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 orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_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'
_cell_length_a 7.6080(2)
_cell_length_b 9.2035(3)
_cell_length_c 13.3936(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 937.83(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 6196
_cell_measurement_temperature 100.02(10)
_cell_measurement_theta_max 73.2220
_cell_measurement_theta_min 4.8020
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.738
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.515
_exptl_absorpt_correction_type 'gaussian and multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.70a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.205
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 368
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -4 0 0.0475
-4 4 0 0.0475
-3 -4 0 0.0831
3 4 0 0.0831
0 -1 9 0.2031
0 1 -9 0.2031
3 3 6 0.1239
3 4 -3 0.1277
-3 -4 3 0.1277
-2 5 3 0.0791
_exptl_crystal_size_max 0.418
_exptl_crystal_size_mid 0.166
_exptl_crystal_size_min 0.095
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.7398 -3.9031 0.1138 -0.9996 0.0257 -0.0091
-3.7398 3.9031 -0.1138 0.9996 -0.0257 0.0091
-3.2647 -4.4827 -0.2615 0.0161 -0.1911 -0.9814
3.2647 4.4827 0.2615 -0.0161 0.1911 0.9814
0.2333 -0.5044 8.6466 -0.0773 0.9776 -0.1960
-0.2333 0.5044 -8.6466 0.0773 -0.9776 0.1960
2.7187 3.2232 5.5524 -0.0605 0.7551 0.6528
2.8488 4.2628 -3.4449 0.0184 -0.2436 0.9697
-2.8488 -4.2628 3.4449 -0.0184 0.2436 -0.9697
-1.7147 5.3276 2.5536 0.8464 0.3515 0.4001
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0250
_diffrn_reflns_av_unetI/netI 0.0150
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 8913
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 73.337
_diffrn_reflns_theta_min 5.833
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.02(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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 -120.00 1.00 1.00 3.00 -- -39.84 -19.00 90.00 121
2 \w 61.00 129.00 1.00 3.00 -- 39.84 178.00 90.00 68
3 \w 61.00 129.00 1.00 3.00 -- 39.84 178.00 0.00 68
4 \w 103.00 178.00 1.00 11.00 -- 107.09 77.00 -30.00 75
5 \w 103.00 178.00 1.00 11.00 -- 107.09 77.00-120.00 75
6 \w 103.00 178.00 1.00 11.00 -- 107.09 77.00 -60.00 75
7 \w 81.00 178.00 1.00 11.00 -- 107.09 45.00 30.00 97
8 \w 34.00 112.00 1.00 11.00 -- 107.09-125.00 30.00 78
9 \w 35.00 136.00 1.00 11.00 -- 107.09 -61.00-150.00 101
10 \w -64.00 34.00 1.00 3.00 -- -39.84 38.00 90.00 98
11 \w -114.00 -15.00 1.00 3.00 -- -39.84 -38.00 0.00 99
12 \w -113.00 -10.00 1.00 3.00 -- -39.84 -67.00 -75.00 103
13 \w 24.00 107.00 1.00 11.00 -- 107.09 -94.00 90.00 83
14 \w 79.00 178.00 1.00 11.00 -- 107.09 30.00 120.00 99
15 \w 54.00 178.00 1.00 11.00 -- 107.09 15.00 -60.00 124
16 \w 78.00 178.00 1.00 11.00 -- 107.09 61.00 150.00 100
17 \w 78.00 178.00 1.00 11.00 -- 107.09 61.00 60.00 100
18 \w 78.00 178.00 1.00 11.00 -- 107.09 61.00-180.00 100
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.1540742000
_diffrn_orient_matrix_UB_12 0.1085300000
_diffrn_orient_matrix_UB_13 0.0015540000
_diffrn_orient_matrix_UB_21 0.0232893000
_diffrn_orient_matrix_UB_22 0.0190494000
_diffrn_orient_matrix_UB_23 0.1135403000
_diffrn_orient_matrix_UB_31 0.1294174000
_diffrn_orient_matrix_UB_32 0.1257819000
_diffrn_orient_matrix_UB_33 -0.0188201000
_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 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.681
_reflns_Friedel_fraction_full 1.000
_reflns_Friedel_fraction_max 0.976
_reflns_number_gt 1829
_reflns_number_total 1869
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_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 1.171.41.70a (Rigaku OD, 2020)'
_computing_data_collection 'CrysAlisPro 1.171.41.70a (Rigaku OD, 2020)'
_computing_data_reduction 'CrysAlisPro 1.171.41.70a (Rigaku OD, 2020)'
_computing_molecular_graphics 'Shelxtl-Plus/XP, Bruker AXS, Inc. 2009'
_computing_publication_material 'Shelxtl-Plus, Bruker AXS, Inc. 2009'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max 0.245
_refine_diff_density_min -0.179
_refine_diff_density_rms 0.040
_refine_ls_abs_structure_details
;
Flack x determined using 736 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.08(6)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.112
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 116
_refine_ls_number_reflns 1869
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0307
_refine_ls_R_factor_gt 0.0300
_refine_ls_restrained_S_all 1.112
_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^)+(0.0471P)^2^+0.1267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0789
_refine_ls_wR_factor_ref 0.0797
_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:
C4(H4), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
C8(H8A,H8B)
2.c Idealised Me refined as rotating group:
C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens mixed
_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
O1 O 0.28352(15) 0.61954(12) 0.53317(7) 0.0209(3) Uani 1 1 d . . . . .
O2 O 0.25407(16) 0.40635(12) 0.46231(8) 0.0251(3) Uani 1 1 d . . . . .
O3 O 0.16161(18) 0.43641(13) 0.80552(8) 0.0273(3) Uani 1 1 d . . . . .
H3 H 0.193(4) 0.493(3) 0.858(2) 0.062(8) Uiso 1 1 d . . . . .
C1 C 0.2392(2) 0.47890(18) 0.53926(11) 0.0198(3) Uani 1 1 d . . . . .
C2 C 0.1829(2) 0.41648(17) 0.63321(11) 0.0206(3) Uani 1 1 d . . . . .
C3 C 0.2002(2) 0.49667(17) 0.71763(11) 0.0202(3) Uani 1 1 d . . . . .
C4 C 0.2709(2) 0.64963(17) 0.71543(10) 0.0205(3) Uani 1 1 d . . . . .
H4 H 0.206301 0.706786 0.767261 0.025 Uiso 1 1 calc R U . . .
C5 C 0.2279(2) 0.71619(16) 0.61380(10) 0.0197(3) Uani 1 1 d . . . . .
H5 H 0.097649 0.729394 0.609217 0.024 Uiso 1 1 calc R U . . .
C6 C 0.1271(2) 0.26019(18) 0.63221(12) 0.0256(4) Uani 1 1 d . . . . .
H6A H 0.016306 0.250741 0.595424 0.038 Uiso 1 1 calc R U . . .
H6B H 0.110493 0.226300 0.700933 0.038 Uiso 1 1 calc R U . . .
H6C H 0.217883 0.201431 0.599624 0.038 Uiso 1 1 calc R U . . .
C7 C 0.4665(2) 0.65031(19) 0.74376(12) 0.0263(4) Uani 1 1 d . . . . .
H7A H 0.533614 0.596256 0.693549 0.039 Uiso 1 1 calc R U . . .
H7B H 0.481669 0.604366 0.809199 0.039 Uiso 1 1 calc R U . . .
H7C H 0.509026 0.750734 0.746594 0.039 Uiso 1 1 calc R U . . .
C8 C 0.3151(2) 0.86095(18) 0.59259(11) 0.0233(4) Uani 1 1 d . . . . .
H8A H 0.444235 0.847613 0.592237 0.028 Uiso 1 1 calc R U . . .
H8B H 0.285849 0.929807 0.646888 0.028 Uiso 1 1 calc R U . . .
C9 C 0.2580(2) 0.92629(18) 0.49279(12) 0.0262(4) Uani 1 1 d . . . . .
H9A H 0.286215 0.858452 0.438718 0.039 Uiso 1 1 calc R U . . .
H9B H 0.320191 1.018173 0.481826 0.039 Uiso 1 1 calc R U . . .
H9C H 0.131042 0.944141 0.493856 0.039 Uiso 1 1 calc R U . . .
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 0.0279(6) 0.0237(5) 0.0111(5) -0.0011(4) 0.0019(4) -0.0001(4)
O2 0.0368(7) 0.0255(6) 0.0131(5) -0.0030(4) 0.0006(5) 0.0009(5)
O3 0.0405(7) 0.0293(6) 0.0120(5) 0.0009(4) 0.0028(5) -0.0055(5)
C1 0.0207(7) 0.0252(8) 0.0136(6) -0.0006(5) -0.0011(6) 0.0016(6)
C2 0.0218(7) 0.0252(8) 0.0147(7) 0.0003(6) -0.0006(6) 0.0008(6)
C3 0.0212(7) 0.0268(8) 0.0126(6) 0.0012(6) 0.0007(6) 0.0010(6)
C4 0.0241(8) 0.0251(7) 0.0124(7) -0.0016(6) 0.0003(6) 0.0002(6)
C5 0.0234(7) 0.0220(7) 0.0137(6) -0.0025(5) 0.0002(6) 0.0013(6)
C6 0.0316(9) 0.0260(8) 0.0193(7) -0.0005(6) 0.0005(6) -0.0042(7)
C7 0.0271(8) 0.0331(9) 0.0187(7) 0.0033(6) -0.0049(7) -0.0030(7)
C8 0.0273(8) 0.0243(8) 0.0184(7) 0.0003(6) -0.0016(6) -0.0011(6)
C9 0.0308(8) 0.0262(8) 0.0215(7) 0.0033(6) -0.0002(6) -0.0005(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
O1 C1 1.340(2) . ?
O1 C5 1.4618(17) . ?
O2 C1 1.2332(19) . ?
O3 H3 0.91(3) . ?
O3 C3 1.3339(18) . ?
C1 C2 1.448(2) . ?
C2 C3 1.357(2) . ?
C2 C6 1.500(2) . ?
C3 C4 1.507(2) . ?
C4 H4 1.0000 . ?
C4 C5 1.5280(19) . ?
C4 C7 1.536(2) . ?
C5 H5 1.0000 . ?
C5 C8 1.515(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.529(2) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
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 C5 118.03(11) . . ?
C3 O3 H3 112.6(19) . . ?
O1 C1 C2 120.69(13) . . ?
O2 C1 O1 116.68(13) . . ?
O2 C1 C2 122.59(14) . . ?
C1 C2 C6 117.16(14) . . ?
C3 C2 C1 118.68(14) . . ?
C3 C2 C6 123.82(14) . . ?
O3 C3 C2 119.21(14) . . ?
O3 C3 C4 118.96(13) . . ?
C2 C3 C4 121.75(13) . . ?
C3 C4 H4 107.6 . . ?
C3 C4 C5 108.39(12) . . ?
C3 C4 C7 110.16(13) . . ?
C5 C4 H4 107.6 . . ?
C5 C4 C7 115.21(13) . . ?
C7 C4 H4 107.6 . . ?
O1 C5 C4 110.62(12) . . ?
O1 C5 H5 108.4 . . ?
O1 C5 C8 105.64(12) . . ?
C4 C5 H5 108.4 . . ?
C8 C5 C4 115.19(13) . . ?
C8 C5 H5 108.4 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.1 . . ?
C5 C8 H8B 109.1 . . ?
C5 C8 C9 112.66(13) . . ?
H8A C8 H8B 107.8 . . ?
C9 C8 H8A 109.1 . . ?
C9 C8 H8B 109.1 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
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
_geom_hbond_publ_flag
O3 H3 O2 0.91(3) 1.72(3) 2.6298(16) 176(3) 2_565 yes
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
O1 C1 C2 C3 -9.5(2) . . . . ?
O1 C1 C2 C6 176.98(14) . . . . ?
O1 C5 C8 C9 61.19(16) . . . . ?
O2 C1 C2 C3 168.28(15) . . . . ?
O2 C1 C2 C6 -5.3(2) . . . . ?
O3 C3 C4 C5 -155.06(14) . . . . ?
O3 C3 C4 C7 78.05(17) . . . . ?
C1 O1 C5 C4 47.98(18) . . . . ?
C1 O1 C5 C8 173.26(13) . . . . ?
C1 C2 C3 O3 -174.85(14) . . . . ?
C1 C2 C3 C4 1.9(2) . . . . ?
C2 C3 C4 C5 28.2(2) . . . . ?
C2 C3 C4 C7 -98.67(17) . . . . ?
C3 C4 C5 O1 -50.78(16) . . . . ?
C3 C4 C5 C8 -170.47(13) . . . . ?
C4 C5 C8 C9 -176.41(14) . . . . ?
C5 O1 C1 O2 165.17(13) . . . . ?
C5 O1 C1 C2 -16.9(2) . . . . ?
C6 C2 C3 O3 -1.8(2) . . . . ?
C6 C2 C3 C4 174.93(14) . . . . ?
C7 C4 C5 O1 73.13(17) . . . . ?
C7 C4 C5 C8 -46.56(18) . . . . ?
_shelx_res_file
;
TITL pf127_a.res in P2(1)2(1)2(1)
p127.res
created by SHELXL-2018/3 at 10:50:58 on 11-Mar-2021
REM Old TITL PF127 in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.112, Rweak 0.022, Alpha 0.001, Orientation as input
REM Flack x = 0.019 ( 0.124 ) from Parsons' quotients
REM Formula found by SHELXT: C9 O3
rem ISOR 0.01 0.02
CELL 1.54184 7.608022 9.203471 13.393645 90 90 90
ZERR 4 0.000204 0.000274 0.000254 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 O
UNIT 36 56 12
EQIV $1 0.5-X,1-Y,0.5+Z
L.S. 4 0 0
PLAN 2
TEMP -173
CONF
HTAB O3 O2_$1
BOND $H
list 4
MORE -1
fmap 2 53
acta
REM
REM
REM
WGHT 0.047100 0.126700
FVAR 6.65927
O1 3 0.283521 0.619543 0.533169 11.00000 0.02787 0.02373 =
0.01108 -0.00108 0.00191 -0.00009
O2 3 0.254069 0.406354 0.462310 11.00000 0.03678 0.02546 =
0.01305 -0.00304 0.00061 0.00087
O3 3 0.161610 0.436407 0.805521 11.00000 0.04054 0.02932 =
0.01200 0.00091 0.00275 -0.00546
H3 2 0.192624 0.493350 0.857876 11.00000 0.06150
C1 1 0.239206 0.478896 0.539257 11.00000 0.02075 0.02517 =
0.01359 -0.00061 -0.00108 0.00164
C2 1 0.182946 0.416479 0.633210 11.00000 0.02180 0.02515 =
0.01473 0.00025 -0.00060 0.00078
C3 1 0.200178 0.496673 0.717635 11.00000 0.02123 0.02685 =
0.01259 0.00119 0.00068 0.00097
C4 1 0.270870 0.649632 0.715426 11.00000 0.02408 0.02515 =
0.01236 -0.00163 0.00032 0.00021
AFIX 13
H4 2 0.206301 0.706786 0.767261 11.00000 -1.20000
AFIX 0
C5 1 0.227864 0.716186 0.613803 11.00000 0.02345 0.02204 =
0.01370 -0.00245 0.00020 0.00127
AFIX 13
H5 2 0.097649 0.729394 0.609217 11.00000 -1.20000
AFIX 0
C6 1 0.127065 0.260194 0.632211 11.00000 0.03160 0.02596 =
0.01928 -0.00051 0.00048 -0.00419
AFIX 137
H6A 2 0.016306 0.250741 0.595424 11.00000 -1.50000
H6B 2 0.110493 0.226300 0.700933 11.00000 -1.50000
H6C 2 0.217883 0.201431 0.599624 11.00000 -1.50000
AFIX 0
C7 1 0.466497 0.650308 0.743756 11.00000 0.02713 0.03310 =
0.01874 0.00327 -0.00486 -0.00296
AFIX 137
H7A 2 0.533614 0.596256 0.693549 11.00000 -1.50000
H7B 2 0.481669 0.604366 0.809199 11.00000 -1.50000
H7C 2 0.509026 0.750734 0.746594 11.00000 -1.50000
AFIX 0
C8 1 0.315114 0.860948 0.592589 11.00000 0.02730 0.02430 =
0.01838 0.00026 -0.00161 -0.00109
AFIX 23
H8A 2 0.444235 0.847613 0.592237 11.00000 -1.20000
H8B 2 0.285849 0.929807 0.646888 11.00000 -1.20000
AFIX 0
C9 1 0.258017 0.926292 0.492792 11.00000 0.03076 0.02620 =
0.02153 0.00332 -0.00023 -0.00050
AFIX 137
H9A 2 0.286215 0.858452 0.438718 11.00000 -1.50000
H9B 2 0.320191 1.018173 0.481826 11.00000 -1.50000
H9C 2 0.131042 0.944141 0.493856 11.00000 -1.50000
AFIX 0
HKLF 4
REM pf127_a.res in P2(1)2(1)2(1)
REM wR2 = 0.0797, GooF = S = 1.112, Restrained GooF = 1.112 for all data
REM R1 = 0.0300 for 1829 Fo > 4sig(Fo) and 0.0307 for all 1869 data
REM 116 parameters refined using 0 restraints
END
WGHT 0.0471 0.1267
REM Highest difference peak 0.245, deepest hole -0.179, 1-sigma level 0.040
Q1 1 0.2301 0.5749 0.7164 11.00000 0.05 0.24
Q2 1 0.3650 0.6467 0.7253 11.00000 0.05 0.19
;
_shelx_res_checksum 36848
_shelx_hkl_file
;
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-7 5 -5 265.085 38.1334 14
7 5 5 271.112 40.9493 13
7 -5 -5 236.608 46.1434 4
-7 5 -6 957.164 68.3210 16
-7 5 -6 1018.17 65.6215 14
7 5 6 1004.99 63.8300 13
7 -5 -6 1006.13 74.6258 4
-7 5 -7 2202.05 92.7678 16
-7 5 -7 2311.68 88.4643 14
7 5 7 2232.30 82.5348 13
7 -5 -7 2400.00 98.4804 4
7 -6 6 570.151 44.2362 6
-7 6 6 487.894 46.2201 18
7 -6 5 149.683 28.0390 6
7 -6 5 149.914 29.9930 4
-7 6 5 152.931 30.7911 18
7 -6 4 1416.73 83.5540 4
7 -6 4 1618.04 80.8436 6
-7 6 4 1585.01 92.8589 18
7 -6 3-12.4169 21.3713 6
-7 6 3-23.1584 26.7503 16
7 -6 3 40.4932 24.1524 4
-7 6 3-6.69807 28.1704 18
7 -6 2 38.2634 20.8857 6
-7 6 2 24.6092 21.8185 16
7 6 -2 13.1890 23.7258 13
7 -6 2 66.1226 25.7141 4
-7 6 2 76.9586 32.1483 18
-7 6 1 1244.35 83.8820 16
7 6 -1 1377.98 83.0428 13
7 -6 1 1291.00 91.0744 4
-7 6 1 1314.34 92.2752 18
-7 6 0 3777.07 147.782 16
7 6 0 3966.24 141.506 13
7 -6 0 3829.83 158.848 4
-7 6 0 3545.67 147.317 18
-7 6 -1 1254.06 86.4994 16
7 6 1 1265.34 80.3198 13
7 -6 -1 1320.76 94.8574 4
-7 6 -1 1103.37 78.4761 18
-7 6 -2 28.9724 22.2738 16
7 6 2 62.1561 28.9469 13
7 -6 -2 34.8438 27.0548 4
-7 6 -2 81.2914 27.0541 18
-7 6 -3 24.7390 25.8624 16
7 6 3 28.6033 25.4594 13
7 -6 -3 1.82748 24.1889 4
-7 6 -4 1608.07 89.9950 16
7 6 4 1578.80 81.1045 13
7 -6 -4 1692.57 96.7684 4
-7 6 -5 174.931 31.9470 16
7 6 5 156.862 30.8370 13
7 -6 -5 166.469 33.1617 4
-7 6 -6 518.486 43.7647 16
7 6 6 471.075 39.1640 13
-7 7 4 672.116 49.9035 18
7 -7 3 468.497 45.3508 4
-7 7 3 417.071 43.6067 18
-7 7 2 964.836 60.6158 16
7 -7 2 1034.96 68.2350 4
-7 7 2 1062.14 67.0992 18
-7 7 1 592.846 52.1442 16
7 7 -1 536.334 44.6577 13
-7 7 1 493.860 48.1398 18
-7 7 0 1175.61 72.7528 16
7 7 0 1073.16 63.2746 13
7 -7 0 1120.15 73.5681 4
-7 7 0 1006.73 62.3062 18
-7 7 -1 602.340 53.3111 16
7 7 1 628.332 48.4258 13
7 -7 -1 511.236 50.7111 4
-7 7 -2 1108.57 69.5583 16
7 7 2 1144.97 63.5246 13
7 -7 -2 1058.02 70.1869 4
-7 7 -3 446.396 44.1894 16
7 7 3 464.806 40.7979 13
7 -7 -3 479.069 46.2369 4
-7 7 -4 664.484 49.1089 16
7 7 4 726.983 46.6386 13
8 0 0 1355.66 108.563 6
8 0 -1 118.936 42.1128 6
8 0 1 237.524 53.7441 6
8 0 -1 185.804 42.6380 4
-8 0 1 176.094 48.7881 18
-8 0 -2 4744.04 160.487 16
8 0 -2 4297.19 181.061 4
8 0 -2 4795.13 204.215 6
8 0 2 4405.23 182.202 6
-8 0 2 4549.18 178.878 18
-8 0 -3 2978.32 126.139 16
8 0 -3 2602.12 140.964 4
8 0 -3 2756.27 156.887 6
8 0 3 2689.42 136.602 6
-8 0 3 2629.37 131.276 18
-8 0 -4 2239.55 109.016 16
8 0 -4 2100.70 126.307 4
8 0 4 1863.28 111.758 6
8 0 5 412.738 53.1084 6
-8 0 -5 493.514 52.4802 16
8 0 -5 559.498 65.5869 4
-8 0 -6 1552.99 85.7593 16
8 0 -6 1746.46 106.215 4
-8 0 -7 835.847 60.1142 16
8 0 -7 793.106 70.1898 4
-8 0 -8 127.823 26.0008 16
8 0 -8 56.2075 20.3279 9
-8 -1 -8 988.688 55.8646 16
-8 -1 -7 1451.77 76.1086 16
8 -1 7 1322.39 72.9500 6
-8 -1 -6 917.638 64.0745 16
8 -1 6 797.655 64.9851 6
-8 -1 -5 669.368 57.6140 16
8 1 -5 813.561 80.8722 4
-8 -1 -4 1784.20 93.9343 16
8 1 -4 1640.56 109.646 4
8 -1 4 1650.07 105.083 6
-8 1 4 1622.70 100.390 18
8 -1 3 125.595 39.6201 6
-8 -1 -3 115.234 31.0790 16
8 1 -3 119.831 40.5723 4
-8 1 3 187.268 43.9537 18
-8 -1 -2 1039.54 71.9813 16
8 1 -2 888.968 79.5155 4
8 1 -2 892.923 96.0103 6
8 -1 2 986.764 90.8953 6
-8 1 2 1007.50 88.7483 18
8 1 -1 481.478 68.9729 6
8 -1 1 505.229 67.1554 6
-8 1 1 405.755 59.8414 18
8 1 0 160.947 46.9124 6
8 -1 0 279.895 55.1831 6
8 -1 0 161.477 40.0833 4
-8 1 0 298.043 54.5292 18
8 1 1 400.324 61.1787 6
8 -1 -1 498.901 68.5401 6
-8 1 -1 523.249 53.6179 16
8 -1 -1 385.252 59.3947 4
-8 1 -2 1049.74 76.7976 16
8 -1 -2 986.017 92.2931 4
8 -1 -2 1047.34 97.3751 6
8 1 2 818.006 81.3846 6
-8 -1 2 875.744 75.9564 18
8 1 3 86.3899 28.7373 6
-8 1 -3 202.275 39.1530 16
8 -1 -3 207.674 49.8284 4
8 -1 -3 101.476 43.5758 6
-8 1 -4 1819.28 99.3913 16
8 -1 -4 1781.06 117.153 4
-8 1 -5 602.375 56.9252 16
8 -1 -5 637.774 72.4736 4
-8 1 -6 894.366 65.7145 16
8 -1 -6 920.361 79.2690 4
-8 1 -7 1474.08 77.2776 16
8 -1 -7 1470.31 91.5466 4
-8 1 -8 1134.44 60.6398 16
8 -1 -8 701.859 54.2443 9
-8 -2 -8 1037.25 54.0496 16
-8 -2 -7 1615.70 75.5378 16
8 -2 7 1437.66 74.2037 6
-8 -2 -6 6249.92 161.258 16
8 -2 6 5766.12 166.890 6
-8 -2 -5 2623.03 107.699 16
8 -2 5 2243.93 111.282 6
-8 2 5 2310.75 110.310 18
-8 -2 -4 2851.65 115.553 16
8 -2 4 2725.26 130.215 6
-8 2 4 2872.75 133.406 18
-8 -2 -3 1723.04 88.2563 16
8 -2 3 1539.75 104.133 6
-8 2 3 1575.05 105.266 18
8 -2 2 5204.24 190.792 6
-8 2 2 5278.47 197.659 18
8 -2 1 2534.99 129.920 4
8 -2 1 2994.12 147.578 6
-8 2 1 2927.35 147.887 18
-8 2 0 856.384 68.4623 16
8 -2 0 763.161 79.1502 4
8 2 0 723.790 79.1339 6
8 -2 0 800.648 79.1378 6
-8 2 0 869.912 83.0324 18
-8 2 -1 2923.81 127.249 16
8 -2 -1 2644.26 142.183 4
8 2 1 2760.13 143.086 6
8 -2 -1 3041.05 151.735 6
-8 2 -1 2939.53 148.984 18
-8 2 -2 5473.65 175.415 16
8 2 2 5026.34 158.633 13
8 -2 -2 5217.18 200.035 4
8 2 2 4939.35 186.094 6
8 -2 -2 5806.07 209.015 6
-8 2 -2 5365.16 196.375 18
-8 2 -3 1808.17 99.5316 16
8 -2 -3 1621.94 113.072 4
8 2 3 1480.82 95.0248 6
8 -2 -3 1673.02 109.351 6
-8 2 -3 1600.42 104.056 18
-8 2 -4 2910.48 125.252 16
8 -2 -4 2951.48 147.945 4
8 -2 -4 2931.18 139.853 6
-8 2 -4 2643.25 127.748 18
-8 2 -5 2422.89 110.280 16
8 -2 -5 2508.36 130.698 4
-8 2 -6 6488.63 170.593 16
8 -2 -6 6361.14 197.030 4
-8 2 -7 1665.91 79.9253 16
8 -2 -7 1636.11 91.2535 4
-8 2 -8 1110.37 57.4714 16
8 -2 -8 1107.55 64.7033 4
-8 -3 -7 4755.46 119.252 16
8 -3 7 4714.27 128.361 6
8 -3 6 65.6629 26.5215 6
-8 3 6 109.858 24.0004 18
-8 -3 -5 861.997 57.8252 16
8 -3 5 829.318 67.7546 6
-8 3 5 877.344 68.9581 18
-8 -3 -4 980.223 63.3070 16
8 -3 4 827.097 68.5454 6
-8 3 4 843.184 72.2881 18
8 -3 3 1024.79 81.3770 6
-8 3 3 1285.27 93.2457 18
8 -3 2 2962.15 132.099 4
8 -3 2 3243.16 143.250 6
-8 3 2 3324.62 150.766 18
8 -3 1 60.6059 29.4082 6
8 -3 1 3.99515 26.5967 4
-8 3 1 15.8315 30.0862 18
-8 3 0 838.716 65.9964 16
8 3 0 858.823 73.3172 13
8 -3 0 748.173 73.2938 4
8 -3 0 884.042 80.2577 6
-8 3 0 829.462 81.5934 18
8 -3 -1-17.9394 30.7249 6
-8 3 -1 62.4074 25.8737 16
8 3 1 7.87328 24.4943 13
8 -3 -1 44.4735 28.7735 4
-8 3 -1 18.6431 30.8373 18
-8 3 -2 3298.13 133.802 16
8 3 2 3284.74 128.035 13
8 -3 -2 3390.88 156.798 4
8 -3 -2 3482.02 149.614 6
-8 3 -2 3342.30 147.946 18
-8 3 -3 1103.20 76.0148 16
8 3 3 1012.15 67.9606 13
8 -3 -3 1086.22 89.6533 4
8 -3 -3 1154.85 83.4163 6
-8 3 -3 1093.38 82.5874 18
-8 3 -4 895.164 68.7919 16
8 3 4 756.304 56.3114 13
8 -3 -4 869.589 78.2138 4
-8 3 -4 718.792 64.1202 18
-8 3 -5 1030.14 69.7318 16
8 -3 -5 902.679 76.1845 4
-8 3 -6 146.716 28.3893 16
8 -3 -6 118.668 31.8836 4
-8 3 -7 5385.47 136.271 16
8 -3 -7 5526.43 152.292 4
8 -4 6 273.997 32.7888 6
-8 -4 -5 967.859 51.8447 16
8 -4 5 1061.21 67.6177 6
-8 4 5 1084.62 67.9986 18
8 -4 4 4824.71 152.094 6
-8 4 4 4865.32 159.115 18
8 -4 3 137.678 31.6614 6
8 -4 3 117.073 30.4962 4
-8 4 3 201.693 39.6776 18
8 -4 2 1434.76 88.9997 4
8 -4 2 1541.62 91.9166 6
-8 4 2 1501.87 97.0313 18
-8 4 1 3782.29 127.924 16
8 -4 1 3440.61 141.441 4
8 -4 1 3830.84 145.495 6
-8 4 1 3796.92 154.676 18
-8 4 0 1121.94 74.2574 16
8 4 0 1066.84 74.4546 13
8 -4 0 1081.20 83.2271 4
8 -4 0 1099.54 77.8049 6
-8 4 0 1133.16 85.3692 18
-8 4 -1 3664.54 135.705 16
8 4 1 3705.57 133.668 13
8 -4 -1 3502.21 148.399 4
8 -4 -1 3833.43 143.449 6
-8 4 -1 3563.60 146.780 18
-8 4 -2 1466.97 85.5176 16
8 4 2 1506.43 83.5978 13
8 -4 -2 1400.74 96.0964 4
8 -4 -2 1630.19 89.9144 6
-8 4 -2 1452.79 89.8597 18
-8 4 -3 167.193 31.0201 16
8 4 3 139.464 30.6857 13
8 -4 -3 142.944 34.9864 4
-8 4 -3 120.669 28.9540 18
-8 4 -4 5186.54 151.931 16
8 4 4 4753.69 130.469 13
8 -4 -4 4824.52 166.630 4
-8 4 -5 1243.10 70.6186 16
8 4 5 1111.37 56.8738 13
8 -4 -5 1166.34 76.0369 4
-8 4 -6 273.560 32.7699 16
8 -4 -6 278.350 35.0606 4
8 -5 4 1560.31 74.3017 6
-8 5 4 1651.50 79.8690 18
8 -5 3 474.073 42.8526 4
8 -5 3 506.497 46.6931 6
-8 5 3 540.883 50.2674 18
8 -5 2 1135.07 70.9529 4
8 -5 2 1261.21 72.4828 6
-8 5 2 1273.61 79.5281 18
-8 5 1 1859.45 82.5044 16
8 -5 1 1800.33 92.6026 4
8 -5 1 1891.16 87.4834 6
-8 5 1 1837.79 95.9391 18
-8 5 0 958.419 62.4250 16
8 -5 0 853.521 67.2697 4
8 -5 0 852.488 62.0806 6
-8 5 0 883.843 65.2317 18
-8 5 -1 1955.85 89.7369 16
8 5 1 1855.18 86.3789 13
8 -5 -1 1713.06 94.5770 4
-8 5 -1 1722.74 89.5503 18
-8 5 -2 1333.09 73.8333 16
8 5 2 1237.08 68.0704 13
8 -5 -2 1177.49 78.2450 4
-8 5 -2 1084.46 66.3023 18
-8 5 -3 546.513 47.3461 16
8 5 3 518.659 46.2371 13
8 -5 -3 491.496 51.3179 4
-8 5 -4 1644.78 75.8466 16
8 5 4 1621.55 68.1626 13
8 -5 -4 1710.60 85.4306 4
-8 5 -5 900.521 52.8359 16
8 -6 0 1000.77 60.2980 4
8 -6 -1 526.991 45.5755 4
-9 0 0 14.2336 22.0316 18
9 0 0-26.4369 27.0944 6
-9 0 1 17.7057 21.6035 18
-9 0 -1 42.7759 22.3865 18
9 0 1-3.08793 25.0503 6
9 0 2 422.918 47.6043 6
-9 0 2 344.474 36.6739 18
-9 0 -2 382.436 44.9339 18
9 0 3 1304.33 75.7343 6
-9 0 -3 1033.59 66.9296 18
-9 0 -4 81.3395 24.2619 18
9 -1 4 323.067 36.3913 6
-9 -1 -4 257.690 33.9490 18
9 -1 3 830.837 60.7620 6
-9 -1 -3 604.720 51.2743 18
9 -1 2 312.481 44.1864 6
-9 1 2 255.495 35.5999 18
9 -1 1 279.842 40.4776 6
-9 1 1 234.654 38.0395 18
-9 -1 -1 259.997 37.6527 18
9 -1 0 119.599 31.0542 6
-9 1 0 82.6529 26.1043 18
-9 -1 0 97.7475 28.4877 18
-9 -1 1 275.041 37.7041 18
-9 1 -1 263.913 38.5347 18
9 -1 -1 276.479 42.8985 6
9 -1 -2 247.732 32.9965 4
-9 1 -2 219.708 34.9349 18
9 -1 -3 718.878 53.3122 4
-9 1 -3 651.411 52.3295 18
9 -1 -4 286.888 32.8189 4
-9 1 -4 209.703 28.3615 18
9 -2 3 3738.76 122.230 6
-9 2 2 1148.70 66.6194 18
-9 -2 -2 833.155 56.5283 18
9 -2 1 816.562 64.7619 6
-9 2 1 722.364 57.6265 18
9 -2 0 66.0849 26.9071 6
-9 2 0 50.6962 19.3963 18
9 -2 -1 632.694 47.5423 4
-9 2 -1 669.674 55.2270 18
9 -2 -2 1279.27 69.0623 4
-9 2 -2 1248.35 71.2341 18
9 -2 -3 3512.83 113.921 4
-9 2 -3 2965.08 104.874 18
9 -3 2 2426.66 92.6140 6
9 -3 1 1355.80 72.6221 6
-9 3 1 1161.95 66.2202 18
9 -3 0 2516.54 98.4005 6
-9 3 0 2199.32 90.7352 18
-9 3 -1 1189.20 65.9017 18
-9 3 -2 1998.99 80.7057 18
0 0 0 0.00 0.00 0
TITL PF127abs in P2(1)2(1)2(1)
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 1.54184 7.608022 9.203471 13.393645 90.0000 90.0000 90.0000
ZERR 4.00 0.000204 0.000274 0.000254 0.0000 0.0000 0.0000
LATT -1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H O
UNIT 36.00 56.00 12.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.1; aver:100.0
TEMP -173
SIZE 0.10 0.17 0.42
TREF
HKLF 4
END
;
_shelx_hkl_checksum 79065
_olex2_date_sample_data_collection 2021-03-10
_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 1.228
_oxdiff_exptl_absorpt_empirical_full_min 0.802