# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2021
#######################################################################
#
# 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.
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data_bzl-69_collect
_database_code_depnum_ccdc_archive 'CCDC 2047909'
loop_
_audit_author_name
_audit_author_address
'Yong-Ming Yan'
;Shenzhen University
China
;
_audit_update_record
;
2020-12-03 deposited with the CCDC. 2021-02-07 downloaded from the CCDC.
;
_audit_creation_date 2020-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common BZL-69
_chemical_name_systematic '(+-)-periplanol A'
_chemical_formula_moiety 'C16 H17 N O5'
_chemical_formula_sum 'C16 H17 N O5'
_chemical_formula_weight 303.30
_chemical_melting_point ?
_chemical_oxdiff_formula 'C136 H136 O40 '
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 15
_space_group_name_H-M_alt 'I 1 2/a 1'
_space_group_name_Hall '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
_cell_length_a 13.3585(3)
_cell_length_b 9.7398(2)
_cell_length_c 21.0467(4)
_cell_angle_alpha 90
_cell_angle_beta 98.944(2)
_cell_angle_gamma 90
_cell_volume 2705.07(10)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 3181
_cell_measurement_temperature 102(4)
_cell_measurement_theta_max 74.0250
_cell_measurement_theta_min 5.0050
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.929
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.54098
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.489
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 1280
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0433
_diffrn_reflns_av_unetI/netI 0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 7210
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 74.192
_diffrn_reflns_theta_min 4.253
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 102(4)
_diffrn_detector 'Pilatus3R 200K-A'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_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 -23.00 31.00 0.50 0.50 -- 0.00 -82.00 150.00 108
2 \w -28.00 19.00 0.50 0.50 -- 0.00 -82.00-150.00 94
3 \w -26.00 20.00 0.50 0.50 -- 0.00 -82.00 30.00 92
4 \w 48.00 123.00 0.50 1.50 -- 95.80 -82.00 120.00 150
5 \w 22.00 60.00 0.50 1.50 -- 95.80 -82.00 -60.00 76
6 \w 89.00 125.00 0.50 1.50 -- 95.80 -82.00 -60.00 72
7 \w 80.00 158.00 0.50 1.50 -- 95.80 45.00 60.00 156
8 \w 73.00 118.00 0.50 1.50 -- 95.80 61.00 90.00 90
9 \w 93.00 183.00 0.50 1.50 -- 95.80 82.00 -30.00 180
10 \w 16.00 41.00 0.50 1.50 -- 95.80 -82.00 120.00 50
11 \w 9.00 110.00 0.50 1.50 -- 95.80 -82.00 -90.00 202
12 \w 16.00 43.00 0.50 1.50 -- 95.80 -82.00 -30.00 54
13 \w 102.00 127.00 0.50 1.50 -- 95.80 -82.00 -30.00 50
14 \w 121.00 185.00 0.50 1.50 -- 95.80 45.00 -90.00 128
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Pro: Kappa single'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0147314000
_diffrn_orient_matrix_UB_12 0.1562747000
_diffrn_orient_matrix_UB_13 0.0079699000
_diffrn_orient_matrix_UB_21 0.0043111000
_diffrn_orient_matrix_UB_22 -0.0150646000
_diffrn_orient_matrix_UB_23 0.0732373000
_diffrn_orient_matrix_UB_31 0.1157366000
_diffrn_orient_matrix_UB_32 -0.0193273000
_diffrn_orient_matrix_UB_33 0.0078824000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'Rotating-anode X-ray tube'
_diffrn_source_type 'MicroMax 007 (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2188
_reflns_number_total 2657
_reflns_odcompleteness_completeness 99.69
_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 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection 'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction 'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.207
_refine_diff_density_min -0.290
_refine_diff_density_rms 0.058
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.085
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 205
_refine_ls_number_reflns 2657
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0643
_refine_ls_R_factor_gt 0.0497
_refine_ls_restrained_S_all 1.085
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+3.2080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1281
_refine_ls_wR_factor_ref 0.1353
_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 O(H) groups
2.a Secondary CH2 refined with riding coordinates:
C3(H3A,H3B), C7(H7A,H7B), C8'(H8'A,H8'B), C8(H8A,H8B), C7'(H7'A,H7'B)
2.b Aromatic/amide H refined with riding coordinates:
C3'(H3'), C6(H6), C6'(H6'), C5'(H5')
2.c Idealised tetrahedral OH refined as rotating group:
O18(H18), O22(H22)
;
_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
O2 O 0.60555(10) 0.40252(14) 0.50656(6) 0.0209(3) Uani 1 1 d . . . . .
O19 O 0.67900(10) 0.61610(14) 0.74693(6) 0.0232(3) Uani 1 1 d . . . . .
O11 O 0.81280(10) 0.41859(15) 0.67761(6) 0.0231(3) Uani 1 1 d . . . . .
O18 O 0.81651(10) 0.65001(15) 0.66935(6) 0.0236(3) Uani 1 1 d . . . . .
H18 H 0.8085 0.6853 0.7036 0.035 Uiso 1 1 calc GR . . . .
O22 O 0.58795(11) -0.00622(18) 0.34576(7) 0.0327(4) Uani 1 1 d . . . . .
H22 H 0.6146 -0.0391 0.3166 0.049 Uiso 1 1 calc GR . . . .
N9 N 0.47863(12) 0.33561(17) 0.59227(7) 0.0200(4) Uani 1 1 d . . . . .
C3 C 0.71298(14) 0.5293(2) 0.58555(8) 0.0192(4) Uani 1 1 d . . . . .
H3A H 0.6741 0.6108 0.5715 0.023 Uiso 1 1 calc R . . . .
H3B H 0.7691 0.5226 0.5615 0.023 Uiso 1 1 calc R . . . .
C4 C 0.64659(14) 0.4028(2) 0.57430(8) 0.0191(4) Uani 1 1 d . . . . .
C1 C 0.66383(14) 0.5480(2) 0.69589(8) 0.0193(4) Uani 1 1 d . . . . .
C2' C 0.53125(14) 0.3058(2) 0.48895(8) 0.0198(4) Uani 1 1 d . . . . .
C1' C 0.46655(14) 0.2686(2) 0.53221(8) 0.0198(4) Uani 1 1 d . . . . .
C3' C 0.51709(14) 0.2530(2) 0.42698(8) 0.0219(4) Uani 1 1 d . . . . .
H3' H 0.5595 0.2805 0.3982 0.026 Uiso 1 1 calc R . . . .
C5 C 0.56135(14) 0.40895(19) 0.61468(8) 0.0189(4) Uani 1 1 d . . . . .
C6 C 0.57291(14) 0.4785(2) 0.67224(8) 0.0205(4) Uani 1 1 d . . . . .
H6 H 0.5198 0.4798 0.6960 0.025 Uiso 1 1 calc R . . . .
C4' C 0.43991(14) 0.1591(2) 0.40752(9) 0.0220(4) Uani 1 1 d . . . . .
C6' C 0.39132(15) 0.1719(2) 0.51413(9) 0.0224(4) Uani 1 1 d . . . . .
H6' H 0.3496 0.1436 0.5431 0.027 Uiso 1 1 calc R . . . .
C7 C 0.71226(14) 0.2760(2) 0.59347(9) 0.0212(4) Uani 1 1 d . . . . .
H7A H 0.6704 0.1941 0.5882 0.025 Uiso 1 1 calc R . . . .
H7B H 0.7634 0.2677 0.5657 0.025 Uiso 1 1 calc R . . . .
C2 C 0.75232(14) 0.5374(2) 0.65704(8) 0.0198(4) Uani 1 1 d . . . . .
C5' C 0.37867(15) 0.1178(2) 0.45223(9) 0.0232(4) Uani 1 1 d . . . . .
H5' H 0.3284 0.0526 0.4403 0.028 Uiso 1 1 calc R . . . .
C8' C 0.48114(15) -0.0294(2) 0.33292(9) 0.0243(4) Uani 1 1 d . . . . .
H8'A H 0.4625 -0.0970 0.3628 0.029 Uiso 1 1 calc R . . . .
H8'B H 0.4627 -0.0651 0.2897 0.029 Uiso 1 1 calc R . . . .
C8 C 0.76346(15) 0.2880(2) 0.66353(9) 0.0235(4) Uani 1 1 d . . . . .
H8A H 0.7129 0.2753 0.6915 0.028 Uiso 1 1 calc R . . . .
H8B H 0.8132 0.2152 0.6727 0.028 Uiso 1 1 calc R . . . .
C7' C 0.42420(16) 0.1031(2) 0.33961(9) 0.0245(4) Uani 1 1 d . . . . .
H7'A H 0.4460 0.1715 0.3112 0.029 Uiso 1 1 calc R . . . .
H7'B H 0.3524 0.0872 0.3259 0.029 Uiso 1 1 calc R . . . .
H9 H 0.4289(19) 0.332(2) 0.6162(12) 0.029(6) Uiso 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O2 0.0202(7) 0.0296(8) 0.0133(6) -0.0015(5) 0.0039(5) -0.0040(5)
O19 0.0250(7) 0.0296(8) 0.0162(6) -0.0029(5) 0.0071(5) -0.0032(6)
O11 0.0196(7) 0.0296(8) 0.0197(6) -0.0015(5) 0.0025(5) 0.0014(6)
O18 0.0219(7) 0.0322(8) 0.0181(6) -0.0066(5) 0.0077(5) -0.0062(6)
O22 0.0248(8) 0.0497(10) 0.0250(7) -0.0095(6) 0.0082(6) 0.0036(7)
N9 0.0181(8) 0.0277(9) 0.0155(7) -0.0016(6) 0.0066(6) -0.0007(6)
C3 0.0191(10) 0.0243(10) 0.0153(8) -0.0005(7) 0.0057(7) -0.0009(7)
C4 0.0185(9) 0.0275(10) 0.0119(8) -0.0003(7) 0.0037(7) 0.0009(7)
C1 0.0198(10) 0.0240(10) 0.0146(8) 0.0014(7) 0.0041(7) 0.0012(7)
C2' 0.0168(9) 0.0252(10) 0.0176(8) -0.0002(7) 0.0033(7) 0.0009(7)
C1' 0.0194(9) 0.0254(10) 0.0149(8) -0.0008(7) 0.0031(7) 0.0021(7)
C3' 0.0207(9) 0.0284(10) 0.0174(8) -0.0006(7) 0.0055(7) 0.0035(8)
C5 0.0175(9) 0.0236(10) 0.0159(8) 0.0014(7) 0.0036(7) 0.0005(7)
C6 0.0190(9) 0.0281(10) 0.0160(8) -0.0004(7) 0.0072(7) 0.0005(7)
C4' 0.0201(10) 0.0271(10) 0.0184(8) -0.0015(7) 0.0015(7) 0.0043(8)
C6' 0.0203(9) 0.0279(11) 0.0194(8) 0.0009(7) 0.0046(7) -0.0002(8)
C7 0.0199(9) 0.0254(10) 0.0194(8) -0.0009(7) 0.0062(7) 0.0010(7)
C2 0.0165(9) 0.0263(10) 0.0169(8) -0.0014(7) 0.0034(7) -0.0017(7)
C5' 0.0210(10) 0.0249(10) 0.0229(9) -0.0028(8) 0.0007(7) -0.0021(8)
C8' 0.0246(10) 0.0303(11) 0.0189(8) -0.0011(8) 0.0065(7) -0.0011(8)
C8 0.0224(10) 0.0286(11) 0.0201(8) 0.0014(8) 0.0052(7) 0.0021(8)
C7' 0.0244(11) 0.0302(11) 0.0183(8) -0.0026(8) 0.0013(8) -0.0007(8)
_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
O2 C4 1.446(2) . ?
O2 C2' 1.377(2) . ?
O19 C1 1.252(2) . ?
O11 C2 1.439(2) . ?
O11 C8 1.442(2) . ?
O18 H18 0.8200 . ?
O18 C2 1.391(2) . ?
O22 H22 0.8200 . ?
O22 C8' 1.428(2) . ?
N9 C1' 1.409(2) . ?
N9 C5 1.339(3) . ?
N9 H9 0.89(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.514(3) . ?
C3 C2 1.517(2) . ?
C4 C5 1.524(2) . ?
C4 C7 1.533(3) . ?
C1 C6 1.412(3) . ?
C1 C2 1.542(2) . ?
C2' C1' 1.397(2) . ?
C2' C3' 1.388(2) . ?
C1' C6' 1.386(3) . ?
C3' H3' 0.9300 . ?
C3' C4' 1.391(3) . ?
C5 C6 1.376(2) . ?
C6 H6 0.9300 . ?
C4' C5' 1.399(3) . ?
C4' C7' 1.513(2) . ?
C6' H6' 0.9300 . ?
C6' C5' 1.391(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.530(2) . ?
C5' H5' 0.9300 . ?
C8' H8'A 0.9700 . ?
C8' H8'B 0.9700 . ?
C8' C7' 1.515(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C7' H7'A 0.9700 . ?
C7' H7'B 0.9700 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2' O2 C4 114.45(14) . . ?
C2 O11 C8 115.49(14) . . ?
C2 O18 H18 109.5 . . ?
C8' O22 H22 109.5 . . ?
C1' N9 H9 119.5(16) . . ?
C5 N9 C1' 122.45(15) . . ?
C5 N9 H9 118.0(16) . . ?
H3A C3 H3B 108.5 . . ?
C4 C3 H3A 110.2 . . ?
C4 C3 H3B 110.2 . . ?
C4 C3 C2 107.57(14) . . ?
C2 C3 H3A 110.2 . . ?
C2 C3 H3B 110.2 . . ?
O2 C4 C3 106.20(14) . . ?
O2 C4 C5 110.38(15) . . ?
O2 C4 C7 111.81(14) . . ?
C3 C4 C5 110.56(15) . . ?
C3 C4 C7 108.49(15) . . ?
C5 C4 C7 109.35(15) . . ?
O19 C1 C6 124.89(16) . . ?
O19 C1 C2 117.08(16) . . ?
C6 C1 C2 118.01(15) . . ?
O2 C2' C1' 119.69(16) . . ?
O2 C2' C3' 119.60(16) . . ?
C3' C2' C1' 120.58(18) . . ?
C2' C1' N9 117.90(17) . . ?
C6' C1' N9 122.54(16) . . ?
C6' C1' C2' 119.52(16) . . ?
C2' C3' H3' 119.8 . . ?
C2' C3' C4' 120.46(17) . . ?
C4' C3' H3' 119.8 . . ?
N9 C5 C4 115.47(15) . . ?
N9 C5 C6 123.14(16) . . ?
C6 C5 C4 121.26(17) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 C1 121.28(16) . . ?
C5 C6 H6 119.4 . . ?
C3' C4' C5' 118.37(17) . . ?
C3' C4' C7' 120.16(17) . . ?
C5' C4' C7' 121.47(18) . . ?
C1' C6' H6' 120.3 . . ?
C1' C6' C5' 119.47(17) . . ?
C5' C6' H6' 120.3 . . ?
C4 C7 H7A 109.6 . . ?
C4 C7 H7B 109.6 . . ?
H7A C7 H7B 108.2 . . ?
C8 C7 C4 110.10(15) . . ?
C8 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
O11 C2 C3 110.36(15) . . ?
O11 C2 C1 109.57(14) . . ?
O18 C2 O11 106.08(15) . . ?
O18 C2 C3 109.55(15) . . ?
O18 C2 C1 110.47(15) . . ?
C3 C2 C1 110.71(15) . . ?
C4' C5' H5' 119.3 . . ?
C6' C5' C4' 121.49(18) . . ?
C6' C5' H5' 119.3 . . ?
O22 C8' H8'A 109.6 . . ?
O22 C8' H8'B 109.6 . . ?
O22 C8' C7' 110.43(17) . . ?
H8'A C8' H8'B 108.1 . . ?
C7' C8' H8'A 109.6 . . ?
C7' C8' H8'B 109.6 . . ?
O11 C8 C7 112.77(15) . . ?
O11 C8 H8A 109.0 . . ?
O11 C8 H8B 109.0 . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C4' C7' C8' 113.36(16) . . ?
C4' C7' H7'A 108.9 . . ?
C4' C7' H7'B 108.9 . . ?
C8' C7' H7'A 108.9 . . ?
C8' C7' H7'B 108.9 . . ?
H7'A C7' H7'B 107.7 . . ?
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 C4 C5 N9 38.3(2) . . . . ?
O2 C4 C5 C6 -145.72(18) . . . . ?
O2 C4 C7 C8 173.79(14) . . . . ?
O2 C2' C1' N9 1.8(3) . . . . ?
O2 C2' C1' C6' 179.49(17) . . . . ?
O2 C2' C3' C4' -177.54(17) . . . . ?
O19 C1 C6 C5 178.16(18) . . . . ?
O19 C1 C2 O11 90.5(2) . . . . ?
O19 C1 C2 O18 -26.0(2) . . . . ?
O19 C1 C2 C3 -147.56(17) . . . . ?
O22 C8' C7' C4' -65.1(2) . . . . ?
N9 C1' C6' C5' 174.93(18) . . . . ?
N9 C5 C6 C1 176.22(18) . . . . ?
C3 C4 C5 N9 155.50(16) . . . . ?
C3 C4 C5 C6 -28.5(2) . . . . ?
C3 C4 C7 C8 57.01(18) . . . . ?
C4 O2 C2' C1' 32.2(2) . . . . ?
C4 O2 C2' C3' -151.98(17) . . . . ?
C4 C3 C2 O11 61.66(18) . . . . ?
C4 C3 C2 O18 178.11(14) . . . . ?
C4 C3 C2 C1 -59.8(2) . . . . ?
C4 C5 C6 C1 0.6(3) . . . . ?
C4 C7 C8 O11 -49.2(2) . . . . ?
C2' O2 C4 C3 -170.86(14) . . . . ?
C2' O2 C4 C5 -51.0(2) . . . . ?
C2' O2 C4 C7 70.98(19) . . . . ?
C2' C1' C6' C5' -2.7(3) . . . . ?
C2' C3' C4' C5' -1.2(3) . . . . ?
C2' C3' C4' C7' 179.31(18) . . . . ?
C1' N9 C5 C4 -6.2(3) . . . . ?
C1' N9 C5 C6 177.88(18) . . . . ?
C1' C2' C3' C4' -1.8(3) . . . . ?
C1' C6' C5' C4' -0.3(3) . . . . ?
C3' C2' C1' N9 -173.96(17) . . . . ?
C3' C2' C1' C6' 3.8(3) . . . . ?
C3' C4' C5' C6' 2.3(3) . . . . ?
C3' C4' C7' C8' 92.0(2) . . . . ?
C5 N9 C1' C2' -15.1(3) . . . . ?
C5 N9 C1' C6' 167.30(18) . . . . ?
C5 C4 C7 C8 -63.6(2) . . . . ?
C6 C1 C2 O11 -88.3(2) . . . . ?
C6 C1 C2 O18 155.18(17) . . . . ?
C6 C1 C2 C3 33.6(2) . . . . ?
C7 C4 C5 N9 -85.1(2) . . . . ?
C7 C4 C5 C6 90.9(2) . . . . ?
C2 O11 C8 C7 49.48(19) . . . . ?
C2 C3 C4 O2 176.65(14) . . . . ?
C2 C3 C4 C5 56.90(19) . . . . ?
C2 C3 C4 C7 -63.01(17) . . . . ?
C2 C1 C6 C5 -3.1(3) . . . . ?
C5' C4' C7' C8' -87.5(2) . . . . ?
C8 O11 C2 O18 -174.30(13) . . . . ?
C8 O11 C2 C3 -55.72(18) . . . . ?
C8 O11 C2 C1 66.44(18) . . . . ?
C7' C4' C5' C6' -178.24(18) . . . . ?
_shelx_res_file
;
bzl-69_collect.res created by SHELXL-2014/7
TITL bzl-69_collect_a.res in I2/a
REM Old TITL BZL-69_collect in I2/a
REM SHELXT solution in I2/a
REM R1 0.130, Rweak 0.117, Alpha 0.026, Orientation as input
REM Formula found by SHELXT: C1 O6
CELL 1.54184 13.3585 9.7398 21.0467 90 98.944 90
ZERR 8 0.0003 0.0002 0.0004 0 0.002 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H N O
UNIT 128 136 8 40
L.S. 4
PLAN 5
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta
OMIT 13 1 12
OMIT 13 3 10
OMIT 9 3 10
REM
REM
REM
WGHT 0.061600 3.208000
FVAR 0.32748
O2 4 0.605549 0.402516 0.506560 11.00000 0.02021 0.02959 =
0.01328 -0.00153 0.00389 -0.00403
O19 4 0.678996 0.616104 0.746928 11.00000 0.02499 0.02961 =
0.01619 -0.00294 0.00714 -0.00316
O11 4 0.812801 0.418591 0.677610 11.00000 0.01964 0.02963 =
0.01970 -0.00151 0.00251 0.00143
O18 4 0.816507 0.650014 0.669355 11.00000 0.02185 0.03221 =
0.01814 -0.00660 0.00773 -0.00621
AFIX 147
H18 2 0.808532 0.685273 0.703592 11.00000 -1.50000
AFIX 0
O22 4 0.587952 -0.006216 0.345760 11.00000 0.02475 0.04971 =
0.02501 -0.00946 0.00816 0.00360
AFIX 147
H22 2 0.614567 -0.039139 0.316647 11.00000 -1.50000
AFIX 0
N9 3 0.478635 0.335614 0.592268 11.00000 0.01811 0.02769 =
0.01547 -0.00165 0.00664 -0.00070
C3 1 0.712982 0.529254 0.585547 11.00000 0.01911 0.02429 =
0.01527 -0.00049 0.00569 -0.00092
AFIX 23
H3A 2 0.674057 0.610828 0.571537 11.00000 -1.20000
H3B 2 0.769081 0.522596 0.561461 11.00000 -1.20000
AFIX 0
C4 1 0.646592 0.402834 0.574303 11.00000 0.01849 0.02748 =
0.01189 -0.00030 0.00373 0.00092
C1 1 0.663832 0.547992 0.695891 11.00000 0.01984 0.02404 =
0.01461 0.00137 0.00411 0.00116
C2' 1 0.531248 0.305792 0.488953 11.00000 0.01677 0.02519 =
0.01756 -0.00024 0.00325 0.00093
C1' 1 0.466550 0.268558 0.532215 11.00000 0.01935 0.02537 =
0.01488 -0.00084 0.00312 0.00213
C3' 1 0.517095 0.252964 0.426977 11.00000 0.02074 0.02840 =
0.01738 -0.00063 0.00554 0.00345
AFIX 43
H3' 2 0.559491 0.280510 0.398245 11.00000 -1.20000
AFIX 0
C5 1 0.561354 0.408947 0.614683 11.00000 0.01748 0.02357 =
0.01588 0.00137 0.00356 0.00052
C6 1 0.572906 0.478536 0.672241 11.00000 0.01900 0.02810 =
0.01598 -0.00042 0.00723 0.00050
AFIX 43
H6 2 0.519785 0.479846 0.696030 11.00000 -1.20000
AFIX 0
C4' 1 0.439914 0.159062 0.407518 11.00000 0.02006 0.02710 =
0.01838 -0.00152 0.00148 0.00432
C6' 1 0.391324 0.171946 0.514125 11.00000 0.02025 0.02791 =
0.01943 0.00085 0.00463 -0.00022
AFIX 43
H6' 2 0.349641 0.143563 0.543133 11.00000 -1.20000
AFIX 0
C7 1 0.712256 0.275960 0.593472 11.00000 0.01990 0.02545 =
0.01935 -0.00094 0.00624 0.00095
AFIX 23
H7A 2 0.670385 0.194142 0.588220 11.00000 -1.20000
H7B 2 0.763449 0.267738 0.565670 11.00000 -1.20000
AFIX 0
C2 1 0.752323 0.537429 0.657038 11.00000 0.01648 0.02629 =
0.01689 -0.00142 0.00345 -0.00169
C5' 1 0.378672 0.117776 0.452230 11.00000 0.02100 0.02489 =
0.02291 -0.00276 0.00067 -0.00210
AFIX 43
H5' 2 0.328350 0.052634 0.440316 11.00000 -1.20000
AFIX 0
C8' 1 0.481140 -0.029368 0.332921 11.00000 0.02458 0.03028 =
0.01895 -0.00112 0.00651 -0.00112
AFIX 23
H8'A 2 0.462452 -0.097049 0.362791 11.00000 -1.20000
H8'B 2 0.462688 -0.065119 0.289669 11.00000 -1.20000
AFIX 0
C8 1 0.763462 0.287981 0.663530 11.00000 0.02244 0.02855 =
0.02006 0.00136 0.00522 0.00214
AFIX 23
H8A 2 0.712939 0.275336 0.691506 11.00000 -1.20000
H8B 2 0.813206 0.215248 0.672730 11.00000 -1.20000
AFIX 0
C7' 1 0.424195 0.103101 0.339613 11.00000 0.02435 0.03025 =
0.01829 -0.00259 0.00131 -0.00069
AFIX 23
H7'A 2 0.446047 0.171502 0.311201 11.00000 -1.20000
H7'B 2 0.352403 0.087217 0.325904 11.00000 -1.20000
AFIX 0
H9 2 0.428937 0.331508 0.616228 11.00000 0.02873
HKLF 4
REM bzl-69_collect_a.res in I2/a
REM R1 = 0.0497 for 2188 Fo > 4sig(Fo) and 0.0643 for all 2657 data
REM 205 parameters refined using 0 restraints
END
WGHT 0.0617 3.2131
REM Highest difference peak 0.207, deepest hole -0.290, 1-sigma level 0.058
Q1 1 0.7349 0.2769 0.6298 11.00000 0.05 0.21
Q2 1 0.5568 0.4861 0.6335 11.00000 0.05 0.19
Q3 1 0.5406 0.2487 0.4692 11.00000 0.05 0.19
Q4 1 0.6260 0.4000 0.5377 11.00000 0.05 0.18
Q5 1 0.4183 0.1317 0.4290 11.00000 0.05 0.18
;
_shelx_res_checksum 65011
_shelx_hkl_file
;
0 0 2 391.38 21.09
0 0 -2 369.12 21.11
0 0 -4 1992.20 111.89
0 0 4 2057.46 111.82
0 0 6 3063.53 168.03
0 0 -6 3030.74 168.16
0 0 -8 1137.39 63.09
0 0 -10 17.85 1.85
0 0 -10 22.49 2.09
0 0 12 6432.18 364.79
0 0 -12 6882.64 364.90
0 0 -14 294.24 16.16
0 0 -14 267.13 16.03
0 0 -16 151.89 8.98
0 0 -16 135.62 8.77
0 0 -18 70.57 5.03
0 0 -18 61.83 4.88
0 0 -20 5.92 2.49
0 0 -20 3.82 2.44
0 0 -22 44.01 3.68
0 0 -22 42.41 3.52
0 0 -24 422.02 23.89
0 0 24 425.31 23.80
0 -1 -1 2311.77 128.26
0 1 1 2345.06 128.26
0 -1 -3 344.45 19.12
0 1 3 337.53 19.07
0 -1 -5 101.43 6.24
0 1 5 99.41 6.05
0 -1 7 266.73 15.20
0 1 7 270.28 15.40
0 -1 -7 271.83 15.42
0 -1 9 171.37 10.35
0 1 -9 219.98 10.99
0 1 -11 1788.54 93.13
0 -1 11 1584.23 93.00
0 1 -11 1652.70 93.06
0 1 -11 1787.70 93.44
0 1 -13 1.86 1.55
0 1 -13 2.63 2.03
0 1 13 0.51 1.39
0 -1 -15 16.21 2.21
0 1 -15 16.19 2.25
0 -1 -15 21.42 2.56
0 1 -15 17.38 2.69
0 1 -17 156.13 9.72
0 1 -17 161.94 9.95
0 -1 -17 163.59 9.85
0 -1 -17 157.01 9.71
0 -1 -19 136.55 8.82
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0 1 -19 139.60 8.88
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0 -1 -21 -0.42 2.06
0 1 -21 2.13 2.26
0 -1 -21 3.12 2.38
0 1 -21 4.02 2.09
0 -1 -23 25.01 2.42
0 -1 23 27.75 2.70
0 1 -23 28.98 2.66
0 -1 -23 29.72 2.80
0 1 -23 28.80 2.73
0 -1 -25 17.16 1.72
0 -1 25 15.88 1.53
0 1 -25 13.62 1.52
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0 -2 -2 3663.03 201.66
0 2 2 3655.95 201.63
0 2 4 668.18 37.28
0 -2 -4 671.14 37.53
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0 -2 -6 1631.55 89.91
0 2 8 226.62 13.37
0 -2 -8 228.56 13.49
0 -2 -10 340.55 18.66
0 2 -10 342.35 18.16
0 -2 -10 375.13 18.26
0 2 10 362.67 18.77
0 2 -10 361.25 18.83
0 -2 -12 75.86 4.98
0 2 -12 76.84 4.92
0 2 -14 0.46 1.61
0 2 -16 36.15 3.17
0 -2 -16 38.32 3.27
0 2 -16 29.56 3.59
0 2 -18 71.91 5.37
0 2 -18 67.96 5.11
0 -2 -18 72.08 5.03
0 -2 20 8.83 2.50
0 -2 -20 7.62 2.06
0 2 -20 8.57 2.23
0 2 -20 7.75 2.62
0 2 -22 19.48 2.65
0 -2 22 21.03 2.59
0 2 -22 16.51 2.29
0 -2 -22 18.42 2.08
0 -2 24 15.26 1.97
0 -2 -24 15.29 1.85
0 -2 -24 17.61 1.96
0 -3 -1 137.75 8.66
0 -3 1 145.00 8.80
0 -3 3 289.62 17.53
0 3 3 305.29 17.11
0 -3 -5 5.27 2.44
0 3 5 4.05 1.66
0 3 7 396.29 21.90
0 3 7 388.99 22.25
0 -3 -7 364.53 22.25
0 3 -9 10.37 1.55
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0 -3 -9 10.37 2.49
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0 3 -11 16.24 2.21
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0 3 -13 189.95 11.60
0 -3 -13 208.69 11.73
0 3 -15 111.46 7.03
0 -3 -15 110.79 7.15
0 -3 -17 20.38 2.70
0 -3 17 17.18 2.81
0 3 -17 16.55 2.50
0 -3 -17 18.08 2.42
0 3 -19 34.38 3.11
0 -3 -19 32.99 3.36
0 -3 -19 32.38 2.88
0 -3 21 26.24 2.89
0 3 -21 22.11 2.92
0 3 -21 19.94 2.41
0 -3 23 0.05 1.73
0 -3 25 5.10 1.29
0 -4 0 130.79 8.41
0 -4 2 14.43 2.86
0 -4 -2 14.39 2.53
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0 -4 -18 29.21 3.14
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15 0 5 9.14 1.35
15 1 -14 5.85 1.16
15 -1 -12 47.70 3.24
15 1 -12 56.90 3.55
15 -1 -10 2.99 1.20
15 1 -10 2.86 1.64
15 -1 -8 -0.24 1.29
15 1 -8 1.08 1.66
15 1 -6 3.70 1.76
15 1 -4 38.00 3.02
15 1 -2 9.08 1.67
15 1 -2 6.07 1.86
15 1 0 56.05 3.80
15 1 0 63.09 3.99
15 1 2 7.59 1.53
15 1 4 8.90 1.39
15 1 6 13.71 1.75
15 2 -13 14.18 1.59
15 2 -11 17.97 1.95
15 2 -9 59.33 4.08
15 2 -7 -0.95 1.78
15 2 -5 -1.63 1.76
15 2 -3 53.88 3.78
15 2 -1 115.04 7.41
15 2 -1 138.15 7.58
15 2 1 1.87 1.73
15 2 3 6.91 1.53
15 2 5 -0.38 1.17
15 3 -8 9.94 1.79
15 3 -6 2.82 1.59
15 3 -4 3.72 1.60
15 3 -2 5.90 1.50
15 3 -2 -1.04 1.86
15 3 0 10.08 1.56
15 3 0 6.15 1.88
15 3 2 19.17 2.00
15 3 4 19.76 1.81
15 4 -11 13.49 1.28
15 4 -9 7.55 1.38
15 -4 -7 2.89 1.05
15 -4 -5 5.06 1.18
15 4 -3 11.23 1.60
15 -4 -3 7.55 1.25
15 4 -1 2.24 1.21
15 4 -1 -0.49 1.56
15 4 1 2.12 1.35
15 4 3 4.52 1.14
15 5 -6 5.41 0.98
15 5 -4 8.31 1.18
15 5 0 2.34 0.97
16 1 -9 76.91 4.60
16 1 -7 82.46 4.92
16 1 -5 6.46 1.10
16 2 -8 -0.05 0.99
16 2 -6 2.37 1.05
16 2 -4 15.75 1.52
16 2 -4 17.29 1.60
16 2 -2 33.93 2.35
16 3 -7 1.69 0.91
16 3 -5 2.08 0.96
16 3 -3 5.83 1.00
0 0 0 0.00 0.00
TITL BZL-69_collect in I2/a
REM I2/a (#15 in standard setting)
CELL 1.54184 13.358495 9.739757 21.046720 90.0000 98.9442 90.0000
ZERR 1.00 0.000343 0.000242 0.000399 0.0000 0.0020 0.0000
LATT 2
SYMM -x+1/2, y,-z
SFAC C H O
UNIT 136.00 136.00 40.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 82381
_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 1.539
_oxdiff_exptl_absorpt_empirical_full_min 0.421
_chemical_compound_source insect
#######################################################################
#
# 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_bzl-82_collect
_database_code_depnum_ccdc_archive 'CCDC 2047910'
loop_
_audit_author_name
_audit_author_address
'Yong-Ming Yan'
;Shenzhen University
China
;
_audit_update_record
;
2020-12-03 deposited with the CCDC. 2021-02-07 downloaded from the CCDC.
;
_audit_creation_date 2020-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common BZL-82
_chemical_name_systematic 'periplactams B and C'
_chemical_formula_moiety '2(C14 H14 N2 O6)'
_chemical_formula_sum 'C28 H28 N4 O12'
_chemical_formula_weight 612.54
_chemical_absolute_configuration ad
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 5.14220(10)
_cell_length_b 35.6110(8)
_cell_length_c 7.3209(2)
_cell_angle_alpha 90
_cell_angle_beta 106.229(2)
_cell_angle_gamma 90
_cell_volume 1287.17(5)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6886
_cell_measurement_temperature 201(140)
_cell_measurement_theta_max 74.0160
_cell_measurement_theta_min 6.2770
_shelx_estimated_absorpt_T_max 0.979
_shelx_estimated_absorpt_T_min 0.901
_exptl_absorpt_coefficient_mu 1.068
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.82705
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.580
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 640
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.02
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0437
_diffrn_reflns_av_unetI/netI 0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -4
_diffrn_reflns_limit_k_max 44
_diffrn_reflns_limit_k_min -43
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 11432
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 75.317
_diffrn_reflns_theta_min 6.297
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 201(140)
_diffrn_detector 'Pilatus3R 200K-A'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.958
_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 -30.00 31.00 0.50 1.00 -- 0.00 -82.00-180.00 122
2 \w -22.00 26.00 0.50 1.00 -- 0.00 -82.00 60.00 96
3 \w -13.00 75.00 0.50 1.00 -- 0.00 57.00 150.00 176
4 \w -15.00 19.00 0.50 1.00 -- 0.00 -82.00 -30.00 68
5 \w -31.00 6.00 0.50 1.00 -- 0.00 -82.00 0.00 74
6 \w 19.00 127.00 0.50 6.50 -- 95.80 -82.00-150.00 216
7 \w 11.00 127.00 0.50 6.50 -- 95.80 -82.00 30.00 232
8 \w 16.00 105.00 0.50 6.50 -- 95.80 -61.00-150.00 178
9 \w 77.00 182.00 0.50 6.50 -- 95.80 45.00 60.00 210
10 \w 18.00 83.00 0.50 6.50 -- 95.80 -77.00 -30.00 130
11 \w 115.00 182.00 0.50 6.50 -- 95.80 45.00 120.00 134
12 \w 6.00 98.00 0.50 6.50 -- 95.80 -30.00 90.00 184
13 \w 70.00 108.00 0.50 6.50 -- 95.80 -82.00 -60.00 76
14 \w 74.00 108.00 0.50 6.50 -- 95.80 -82.00 120.00 68
15 \w 82.00 110.00 0.50 6.50 -- 95.80 -61.00 90.00 56
16 \w 6.00 34.00 0.50 6.50 -- 95.80 -61.00 90.00 56
17 \w 85.00 178.00 0.50 6.50 -- 95.80 30.00-120.00 186
18 \w 115.00 183.00 0.50 6.50 -- 95.80 30.00 -30.00 136
19 \w 12.00 119.00 0.50 6.50 -- 95.80 -61.00 30.00 214
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0231475000
_diffrn_orient_matrix_UB_12 -0.0431401000
_diffrn_orient_matrix_UB_13 0.0018301000
_diffrn_orient_matrix_UB_21 -0.1600373000
_diffrn_orient_matrix_UB_22 -0.0011368000
_diffrn_orient_matrix_UB_23 -0.2120474000
_diffrn_orient_matrix_UB_31 0.2667827000
_diffrn_orient_matrix_UB_32 0.0030472000
_diffrn_orient_matrix_UB_33 -0.0556111000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'Rotating-anode X-ray tube'
_diffrn_source_type 'MicroMax 007 (Cu) X-ray Source'
_reflns_Friedel_coverage 0.896
_reflns_Friedel_fraction_full 0.954
_reflns_Friedel_fraction_max 0.888
_reflns_number_gt 4399
_reflns_number_total 4938
_reflns_odcompleteness_completeness 98.81
_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 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection 'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction 'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.464
_refine_diff_density_min -0.342
_refine_diff_density_rms 0.089
_refine_ls_abs_structure_details
;
Flack x determined using 1816 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.08(14)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 403
_refine_ls_number_reflns 4938
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0667
_refine_ls_R_factor_gt 0.0594
_refine_ls_restrained_S_all 1.042
_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^)+(0.0974P)^2^+1.5534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1579
_refine_ls_wR_factor_ref 0.1663
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
C5'A(H5'A), C3(H3), C5'(H5'), C3A(H3A)
2.b Secondary CH2 refined with riding coordinates:
C6'(H6'A,H6'B), C6'A(H6'C,H6'D), C4A(H4AA,H4AB), C4(H4A,H4B)
2.c Aromatic/amide H refined with riding coordinates:
N2'(H2'), N2'A(H2'A), N4'A(H4'A), N4'(H4'), C5A(H5A), C5(H5)
2.d Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C11A(H11D,H11E,H11F)
2.e Idealised tetrahedral OH refined as rotating group:
O21(H21), O43(H43), O41(H41), O19(H19)
;
_atom_sites_solution_hydrogens geom
_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
O21 O 0.6263(8) 0.58955(12) 0.8636(6) 0.0245(9) Uani 1 1 d . . . . .
H21 H 0.4953 0.5801 0.7868 0.037 Uiso 1 1 calc GR . . . .
O17 O 0.6649(8) 0.47432(12) 0.5647(6) 0.0253(9) Uani 1 1 d . . . . .
O2 O 1.3891(8) 0.71006(12) 0.6365(6) 0.0238(9) Uani 1 1 d . . . . .
O39 O 0.8260(8) 0.45851(12) 1.1351(6) 0.0243(9) Uani 1 1 d . . . . .
O2A O -0.4450(9) 0.29064(12) 0.7984(6) 0.0273(9) Uani 1 1 d . . . . .
O43 O 0.1128(9) 0.42059(12) 0.4435(6) 0.0272(10) Uani 1 1 d . . . . .
H43 H -0.0013 0.4237 0.3411 0.041 Uiso 1 1 calc GR . . . .
O20 O 1.1655(9) 0.68990(12) 0.3518(6) 0.0268(9) Uani 1 1 d . . . . .
O41 O 0.1815(9) 0.36538(13) 1.0377(6) 0.0271(9) Uani 1 1 d . . . . .
H41 H 0.1099 0.3491 1.0862 0.041 Uiso 1 1 calc GR . . . .
O40 O 0.2366(8) 0.53826(12) 0.7316(6) 0.0242(9) Uani 1 1 d . . . . .
O18 O 0.0662(8) 0.54878(13) 0.1375(6) 0.0279(10) Uani 1 1 d . . . . .
O19 O 0.7591(9) 0.64481(12) 0.3053(5) 0.0255(9) Uani 1 1 d . . . . .
H19 H 0.8629 0.6594 0.2744 0.038 Uiso 1 1 calc GR . . . .
O42 O -0.1288(9) 0.30927(13) 1.0506(6) 0.0312(10) Uani 1 1 d . . . . .
N2' N 0.3221(9) 0.50412(14) 0.3355(7) 0.0210(10) Uani 1 1 d . . . . .
H2' H 0.2118 0.4855 0.3063 0.025 Uiso 1 1 calc R . . . .
N2'A N 0.5783(9) 0.50611(13) 0.9547(6) 0.0205(10) Uani 1 1 d . . . . .
H2'A H 0.6957 0.5239 0.9848 0.025 Uiso 1 1 calc R . . . .
N4'A N 0.1894(9) 0.47744(14) 0.8247(7) 0.0202(9) Uani 1 1 d . . . . .
H4'A H 0.0234 0.4739 0.7612 0.024 Uiso 1 1 calc R . . . .
N4' N 0.6902(10) 0.53599(13) 0.4744(7) 0.0218(10) Uani 1 1 d . . . . .
H4' H 0.8487 0.5414 0.5466 0.026 Uiso 1 1 calc R . . . .
C3' C 0.5743(11) 0.50230(17) 0.4702(8) 0.0203(11) Uani 1 1 d . . . . .
C8 C 0.8279(11) 0.64186(17) 0.4961(8) 0.0198(11) Uani 1 1 d . . . . .
C9 C 1.0483(11) 0.66252(16) 0.6121(8) 0.0209(12) Uani 1 1 d . . . . .
C8A C 0.0607(11) 0.36663(17) 0.8486(8) 0.0191(11) Uani 1 1 d . . . . .
C6 C 0.7574(12) 0.61210(16) 0.7716(8) 0.0220(12) Uani 1 1 d . . . . .
C9A C -0.1567(11) 0.34195(16) 0.7640(8) 0.0203(11) Uani 1 1 d . . . . .
C3'A C 0.3194(11) 0.50976(16) 0.8254(8) 0.0196(11) Uani 1 1 d . . . . .
C1 C 1.2009(11) 0.68795(17) 0.5247(8) 0.0221(11) Uani 1 1 d . . . . .
C6A C 0.0244(11) 0.39459(16) 0.5455(8) 0.0214(11) Uani 1 1 d . . . . .
C1' C 0.2705(11) 0.53883(17) 0.2554(8) 0.0211(11) Uani 1 1 d . . . . .
C10 C 1.1200(12) 0.65684(16) 0.8100(8) 0.0210(12) Uani 1 1 d . . . . .
C5'A C 0.3565(11) 0.44893(16) 0.9421(8) 0.0187(11) Uani 1 1 d . . . . .
H5'A H 0.2776 0.4409 1.0431 0.022 Uiso 1 1 calc R . . . .
C7A C 0.1572(11) 0.39223(16) 0.7392(8) 0.0215(12) Uani 1 1 d . . . . .
C10A C -0.2702(11) 0.34315(17) 0.5661(8) 0.0225(12) Uani 1 1 d . . . . .
C7 C 0.6792(11) 0.61702(16) 0.5731(8) 0.0192(11) Uani 1 1 d . . . . .
C1'A C 0.6177(11) 0.47062(15) 1.0256(7) 0.0180(11) Uani 1 1 d . . . . .
C1A C -0.2395(12) 0.31339(18) 0.8800(9) 0.0238(12) Uani 1 1 d . . . . .
C3 C 1.3969(11) 0.71508(18) 0.8385(8) 0.0220(12) Uani 1 1 d . . . . .
H3 H 1.2518 0.7323 0.8471 0.026 Uiso 1 1 calc R . . . .
C5A C -0.1884(12) 0.37013(17) 0.4588(8) 0.0224(12) Uani 1 1 d . . . . .
H5A H -0.2740 0.3721 0.3293 0.027 Uiso 1 1 calc R . . . .
C5 C 0.9816(12) 0.63159(17) 0.8875(8) 0.0211(11) Uani 1 1 d . . . . .
H5 H 1.0358 0.6272 1.0179 0.025 Uiso 1 1 calc R . . . .
C5' C 0.5194(11) 0.56261(16) 0.3438(8) 0.0220(12) Uani 1 1 d . . . . .
H5' H 0.6061 0.5706 0.2468 0.026 Uiso 1 1 calc R . . . .
C6' C 0.4370(12) 0.59713(16) 0.4434(8) 0.0222(12) Uani 1 1 d . . . . .
H6'A H 0.3376 0.6146 0.3476 0.027 Uiso 1 1 calc R . . . .
H6'B H 0.3174 0.5890 0.5174 0.027 Uiso 1 1 calc R . . . .
C11 C 1.6686(12) 0.73317(18) 0.9296(9) 0.0260(12) Uani 1 1 d . . . . .
H11A H 1.8107 0.7172 0.9132 0.039 Uiso 1 1 calc GR . . . .
H11B H 1.6896 0.7368 1.0629 0.039 Uiso 1 1 calc GR . . . .
H11C H 1.6777 0.7570 0.8706 0.039 Uiso 1 1 calc GR . . . .
C6'A C 0.4084(11) 0.41485(16) 0.8284(8) 0.0200(11) Uani 1 1 d . . . . .
H6'C H 0.4849 0.4235 0.7289 0.024 Uiso 1 1 calc R . . . .
H6'D H 0.5411 0.3987 0.9124 0.024 Uiso 1 1 calc R . . . .
C3A C -0.6282(12) 0.30058(17) 0.6119(9) 0.0238(12) Uani 1 1 d . . . . .
H3A H -0.7438 0.3214 0.6294 0.029 Uiso 1 1 calc R . . . .
C4A C -0.4724(12) 0.31308(18) 0.4780(8) 0.0234(12) Uani 1 1 d . . . . .
H4AA H -0.5972 0.3227 0.3624 0.028 Uiso 1 1 calc R . . . .
H4AB H -0.3782 0.2918 0.4440 0.028 Uiso 1 1 calc R . . . .
C4 C 1.3616(12) 0.67808(16) 0.9281(8) 0.0220(12) Uani 1 1 d . . . . .
H4A H 1.5232 0.6630 0.9431 0.026 Uiso 1 1 calc R . . . .
H4B H 1.3393 0.6825 1.0536 0.026 Uiso 1 1 calc R . . . .
C11A C -0.8045(12) 0.26673(18) 0.5445(9) 0.0268(13) Uani 1 1 d . . . . .
H11D H -0.6923 0.2452 0.5437 0.040 Uiso 1 1 calc GR . . . .
H11E H -0.9187 0.2712 0.4182 0.040 Uiso 1 1 calc GR . . . .
H11F H -0.9147 0.2622 0.6286 0.040 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
O21 0.022(2) 0.029(2) 0.0198(19) 0.0036(16) 0.0014(16) -0.0062(17)
O17 0.024(2) 0.023(2) 0.025(2) 0.0027(17) 0.0018(16) -0.0001(16)
O2 0.024(2) 0.029(2) 0.0189(19) -0.0009(16) 0.0072(16) -0.0051(17)
O39 0.020(2) 0.027(2) 0.0218(19) 0.0021(17) 0.0002(16) -0.0012(16)
O2A 0.026(2) 0.030(2) 0.023(2) 0.0022(17) 0.0026(17) -0.0071(17)
O43 0.026(2) 0.030(2) 0.021(2) 0.0058(17) -0.0008(17) -0.0081(17)
O20 0.033(2) 0.030(2) 0.0172(19) -0.0004(17) 0.0057(16) -0.0021(18)
O41 0.031(2) 0.031(2) 0.0174(18) 0.0048(17) 0.0022(16) -0.0074(18)
O40 0.026(2) 0.022(2) 0.0211(19) 0.0038(16) 0.0007(16) 0.0016(16)
O18 0.024(2) 0.029(2) 0.025(2) -0.0011(17) -0.0042(16) -0.0020(17)
O19 0.029(2) 0.030(2) 0.0147(18) 0.0035(17) 0.0016(16) -0.0013(17)
O42 0.035(2) 0.033(2) 0.022(2) 0.0044(18) 0.0025(18) -0.0065(19)
N2' 0.013(2) 0.025(3) 0.025(2) -0.002(2) 0.0055(18) -0.0044(19)
N2'A 0.022(2) 0.019(2) 0.017(2) 0.0012(19) -0.0002(18) -0.0029(19)
N4'A 0.015(2) 0.022(2) 0.023(2) 0.0005(19) 0.0033(18) -0.0007(17)
N4' 0.016(2) 0.020(2) 0.026(2) -0.003(2) 0.0002(18) -0.0009(18)
C3' 0.018(3) 0.025(3) 0.018(3) -0.003(2) 0.006(2) 0.000(2)
C8 0.018(3) 0.025(3) 0.016(2) -0.002(2) 0.004(2) 0.005(2)
C9 0.020(3) 0.023(3) 0.020(3) 0.002(2) 0.005(2) 0.001(2)
C8A 0.013(2) 0.024(3) 0.020(3) 0.000(2) 0.005(2) 0.003(2)
C6 0.023(3) 0.021(3) 0.022(3) 0.004(2) 0.005(2) 0.002(2)
C9A 0.017(3) 0.023(3) 0.021(3) 0.001(2) 0.005(2) 0.000(2)
C3'A 0.022(3) 0.021(3) 0.017(3) -0.003(2) 0.007(2) 0.001(2)
C1 0.021(3) 0.023(3) 0.021(3) -0.001(2) 0.004(2) 0.002(2)
C6A 0.019(3) 0.019(3) 0.025(3) 0.001(2) 0.004(2) -0.001(2)
C1' 0.017(3) 0.022(3) 0.024(3) -0.005(2) 0.006(2) 0.000(2)
C10 0.021(3) 0.020(3) 0.019(3) -0.001(2) 0.002(2) 0.001(2)
C5'A 0.012(3) 0.022(3) 0.023(3) 0.003(2) 0.006(2) -0.002(2)
C7A 0.019(3) 0.020(3) 0.023(3) -0.003(2) 0.003(2) 0.001(2)
C10A 0.015(3) 0.027(3) 0.024(3) -0.004(2) 0.003(2) 0.003(2)
C7 0.018(3) 0.020(3) 0.020(3) 0.000(2) 0.005(2) 0.003(2)
C1'A 0.017(3) 0.022(3) 0.017(2) 0.000(2) 0.006(2) 0.000(2)
C1A 0.019(3) 0.024(3) 0.025(3) -0.006(2) 0.002(2) -0.001(2)
C3 0.017(3) 0.030(3) 0.021(3) -0.003(2) 0.008(2) 0.000(2)
C5A 0.023(3) 0.024(3) 0.017(2) 0.001(2) 0.000(2) -0.001(2)
C5 0.022(3) 0.024(3) 0.016(2) 0.002(2) 0.002(2) 0.000(2)
C5' 0.019(3) 0.022(3) 0.022(3) -0.001(2) 0.001(2) -0.001(2)
C6' 0.022(3) 0.022(3) 0.019(3) -0.001(2) 0.002(2) 0.000(2)
C11 0.027(3) 0.025(3) 0.026(3) -0.006(2) 0.008(2) -0.004(2)
C6'A 0.017(3) 0.022(3) 0.020(3) -0.001(2) 0.004(2) 0.000(2)
C3A 0.021(3) 0.024(3) 0.026(3) -0.002(2) 0.006(2) -0.001(2)
C4A 0.020(3) 0.026(3) 0.023(3) -0.002(2) 0.004(2) -0.001(2)
C4 0.023(3) 0.024(3) 0.018(3) -0.002(2) 0.004(2) -0.001(2)
C11A 0.020(3) 0.030(3) 0.030(3) -0.003(2) 0.006(2) -0.002(2)
_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
O21 H21 0.8200 . ?
O21 C6 1.344(7) . ?
O17 C3' 1.228(7) . ?
O2 C1 1.335(7) . ?
O2 C3 1.479(7) . ?
O39 C1'A 1.223(7) . ?
O2A C1A 1.333(7) . ?
O2A C3A 1.469(7) . ?
O43 H43 0.8200 . ?
O43 C6A 1.346(7) . ?
O20 C1 1.229(7) . ?
O41 H41 0.8200 . ?
O41 C8A 1.350(7) . ?
O40 C3'A 1.233(7) . ?
O18 C1' 1.211(7) . ?
O19 H19 0.8200 . ?
O19 C8 1.346(6) . ?
O42 C1A 1.228(7) . ?
N2' H2' 0.8600 . ?
N2' C3' 1.394(7) . ?
N2' C1' 1.362(8) . ?
N2'A H2'A 0.8600 . ?
N2'A C3'A 1.408(7) . ?
N2'A C1'A 1.359(7) . ?
N4'A H4'A 0.8600 . ?
N4'A C3'A 1.331(8) . ?
N4'A C5'A 1.447(7) . ?
N4' H4' 0.8600 . ?
N4' C3' 1.336(8) . ?
N4' C5' 1.454(7) . ?
C8 C9 1.418(8) . ?
C8 C7 1.387(8) . ?
C9 C1 1.458(8) . ?
C9 C10 1.407(8) . ?
C8A C9A 1.421(8) . ?
C8A C7A 1.394(8) . ?
C6 C7 1.406(8) . ?
C6 C5 1.409(8) . ?
C9A C10A 1.403(8) . ?
C9A C1A 1.462(8) . ?
C6A C7A 1.394(8) . ?
C6A C5A 1.404(8) . ?
C1' C5' 1.520(8) . ?
C10 C5 1.365(8) . ?
C10 C4 1.504(8) . ?
C5'A H5'A 0.9800 . ?
C5'A C1'A 1.522(7) . ?
C5'A C6'A 1.537(8) . ?
C7A C6'A 1.507(8) . ?
C10A C5A 1.379(8) . ?
C10A C4A 1.506(8) . ?
C7 C6' 1.515(8) . ?
C3 H3 0.9800 . ?
C3 C11 1.514(8) . ?
C3 C4 1.506(8) . ?
C5A H5A 0.9300 . ?
C5 H5 0.9300 . ?
C5' H5' 0.9800 . ?
C5' C6' 1.548(8) . ?
C6' H6'A 0.9700 . ?
C6' H6'B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C6'A H6'C 0.9700 . ?
C6'A H6'D 0.9700 . ?
C3A H3A 0.9800 . ?
C3A C4A 1.497(8) . ?
C3A C11A 1.506(8) . ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C11A H11D 0.9600 . ?
C11A H11E 0.9600 . ?
C11A H11F 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
C6 O21 H21 109.5 . . ?
C1 O2 C3 119.7(4) . . ?
C1A O2A C3A 119.5(5) . . ?
C6A O43 H43 109.5 . . ?
C8A O41 H41 109.5 . . ?
C8 O19 H19 109.5 . . ?
C3' N2' H2' 123.9 . . ?
C1' N2' H2' 123.9 . . ?
C1' N2' C3' 112.2(5) . . ?
C3'A N2'A H2'A 124.6 . . ?
C1'A N2'A H2'A 124.6 . . ?
C1'A N2'A C3'A 110.8(5) . . ?
C3'A N4'A H4'A 123.5 . . ?
C3'A N4'A C5'A 113.0(5) . . ?
C5'A N4'A H4'A 123.5 . . ?
C3' N4' H4' 123.6 . . ?
C3' N4' C5' 112.8(5) . . ?
C5' N4' H4' 123.6 . . ?
O17 C3' N2' 124.6(5) . . ?
O17 C3' N4' 128.3(5) . . ?
N4' C3' N2' 107.2(5) . . ?
O19 C8 C9 121.0(5) . . ?
O19 C8 C7 117.2(5) . . ?
C7 C8 C9 121.8(5) . . ?
C8 C9 C1 119.9(5) . . ?
C10 C9 C8 118.5(5) . . ?
C10 C9 C1 121.5(5) . . ?
O41 C8A C9A 120.5(5) . . ?
O41 C8A C7A 118.4(5) . . ?
C7A C8A C9A 121.2(5) . . ?
O21 C6 C7 123.6(5) . . ?
O21 C6 C5 115.7(5) . . ?
C7 C6 C5 120.7(5) . . ?
C8A C9A C1A 119.9(5) . . ?
C10A C9A C8A 118.7(5) . . ?
C10A C9A C1A 121.1(5) . . ?
O40 C3'A N2'A 124.4(5) . . ?
O40 C3'A N4'A 128.0(5) . . ?
N4'A C3'A N2'A 107.6(5) . . ?
O2 C1 C9 119.0(5) . . ?
O20 C1 O2 118.1(5) . . ?
O20 C1 C9 122.9(5) . . ?
O43 C6A C7A 117.4(5) . . ?
O43 C6A C5A 121.2(5) . . ?
C7A C6A C5A 121.4(5) . . ?
O18 C1' N2' 126.7(5) . . ?
O18 C1' C5' 126.9(6) . . ?
N2' C1' C5' 106.4(5) . . ?
C9 C10 C4 117.2(5) . . ?
C5 C10 C9 120.4(5) . . ?
C5 C10 C4 122.4(5) . . ?
N4'A C5'A H5'A 110.5 . . ?
N4'A C5'A C1'A 101.1(4) . . ?
N4'A C5'A C6'A 113.4(5) . . ?
C1'A C5'A H5'A 110.5 . . ?
C1'A C5'A C6'A 110.5(4) . . ?
C6'A C5'A H5'A 110.5 . . ?
C8A C7A C6A 118.2(5) . . ?
C8A C7A C6'A 120.0(5) . . ?
C6A C7A C6'A 121.7(5) . . ?
C9A C10A C4A 117.3(5) . . ?
C5A C10A C9A 120.3(5) . . ?
C5A C10A C4A 122.4(5) . . ?
C8 C7 C6 117.9(5) . . ?
C8 C7 C6' 119.6(5) . . ?
C6 C7 C6' 122.5(5) . . ?
O39 C1'A N2'A 126.0(5) . . ?
O39 C1'A C5'A 126.7(5) . . ?
N2'A C1'A C5'A 107.3(4) . . ?
O2A C1A C9A 119.0(5) . . ?
O42 C1A O2A 117.9(6) . . ?
O42 C1A C9A 123.1(5) . . ?
O2 C3 H3 109.3 . . ?
O2 C3 C11 104.8(4) . . ?
O2 C3 C4 110.9(5) . . ?
C11 C3 H3 109.3 . . ?
C4 C3 H3 109.3 . . ?
C4 C3 C11 112.9(5) . . ?
C6A C5A H5A 120.1 . . ?
C10A C5A C6A 119.9(5) . . ?
C10A C5A H5A 120.1 . . ?
C6 C5 H5 119.7 . . ?
C10 C5 C6 120.6(5) . . ?
C10 C5 H5 119.7 . . ?
N4' C5' C1' 101.5(5) . . ?
N4' C5' H5' 110.6 . . ?
N4' C5' C6' 113.7(5) . . ?
C1' C5' H5' 110.6 . . ?
C1' C5' C6' 109.5(5) . . ?
C6' C5' H5' 110.6 . . ?
C7 C6' C5' 112.4(5) . . ?
C7 C6' H6'A 109.1 . . ?
C7 C6' H6'B 109.1 . . ?
C5' C6' H6'A 109.1 . . ?
C5' C6' H6'B 109.1 . . ?
H6'A C6' H6'B 107.9 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C5'A C6'A H6'C 108.9 . . ?
C5'A C6'A H6'D 108.9 . . ?
C7A C6'A C5'A 113.5(5) . . ?
C7A C6'A H6'C 108.9 . . ?
C7A C6'A H6'D 108.9 . . ?
H6'C C6'A H6'D 107.7 . . ?
O2A C3A H3A 108.4 . . ?
O2A C3A C4A 111.0(5) . . ?
O2A C3A C11A 106.4(5) . . ?
C4A C3A H3A 108.4 . . ?
C4A C3A C11A 114.0(5) . . ?
C11A C3A H3A 108.4 . . ?
C10A C4A H4AA 109.4 . . ?
C10A C4A H4AB 109.4 . . ?
C3A C4A C10A 111.2(5) . . ?
C3A C4A H4AA 109.4 . . ?
C3A C4A H4AB 109.4 . . ?
H4AA C4A H4AB 108.0 . . ?
C10 C4 C3 111.7(5) . . ?
C10 C4 H4A 109.3 . . ?
C10 C4 H4B 109.3 . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C3A C11A H11D 109.5 . . ?
C3A C11A H11E 109.5 . . ?
C3A C11A H11F 109.5 . . ?
H11D C11A H11E 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 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
O21 C6 C7 C8 178.4(5) . . . . ?
O21 C6 C7 C6' 0.1(9) . . . . ?
O21 C6 C5 C10 -176.3(5) . . . . ?
O2 C3 C4 C10 -50.2(6) . . . . ?
O2A C3A C4A C10A -51.3(7) . . . . ?
O43 C6A C7A C8A 177.2(5) . . . . ?
O43 C6A C7A C6'A -6.4(8) . . . . ?
O43 C6A C5A C10A 178.4(5) . . . . ?
O41 C8A C9A C10A -177.6(5) . . . . ?
O41 C8A C9A C1A -3.9(8) . . . . ?
O41 C8A C7A C6A -177.2(5) . . . . ?
O41 C8A C7A C6'A 6.3(8) . . . . ?
O18 C1' C5' N4' 179.0(6) . . . . ?
O18 C1' C5' C6' 58.5(8) . . . . ?
O19 C8 C9 C1 1.2(8) . . . . ?
O19 C8 C9 C10 -176.7(5) . . . . ?
O19 C8 C7 C6 176.7(5) . . . . ?
O19 C8 C7 C6' -4.9(8) . . . . ?
N2' C1' C5' N4' -0.8(6) . . . . ?
N2' C1' C5' C6' -121.3(5) . . . . ?
N4'A C5'A C1'A O39 -179.5(5) . . . . ?
N4'A C5'A C1'A N2'A 0.1(5) . . . . ?
N4'A C5'A C6'A C7A -66.5(6) . . . . ?
N4' C5' C6' C7 53.8(7) . . . . ?
C3' N2' C1' O18 -178.4(6) . . . . ?
C3' N2' C1' C5' 1.3(6) . . . . ?
C3' N4' C5' C1' 0.0(6) . . . . ?
C3' N4' C5' C6' 117.4(5) . . . . ?
C8 C9 C1 O2 173.1(5) . . . . ?
C8 C9 C1 O20 -7.4(9) . . . . ?
C8 C9 C10 C5 0.8(8) . . . . ?
C8 C9 C10 C4 177.7(5) . . . . ?
C8 C7 C6' C5' 80.9(7) . . . . ?
C9 C8 C7 C6 -1.4(8) . . . . ?
C9 C8 C7 C6' 177.0(5) . . . . ?
C9 C10 C5 C6 -2.9(9) . . . . ?
C9 C10 C4 C3 30.0(7) . . . . ?
C8A C9A C10A C5A -5.9(8) . . . . ?
C8A C9A C10A C4A 171.5(5) . . . . ?
C8A C9A C1A O2A 179.6(5) . . . . ?
C8A C9A C1A O42 -0.2(9) . . . . ?
C8A C7A C6'A C5'A -80.0(7) . . . . ?
C6 C7 C6' C5' -100.8(6) . . . . ?
C9A C8A C7A C6A 3.7(8) . . . . ?
C9A C8A C7A C6'A -172.8(5) . . . . ?
C9A C10A C5A C6A 5.1(9) . . . . ?
C9A C10A C4A C3A 31.3(7) . . . . ?
C3'A N2'A C1'A O39 177.0(5) . . . . ?
C3'A N2'A C1'A C5'A -2.5(6) . . . . ?
C3'A N4'A C5'A C1'A 2.6(6) . . . . ?
C3'A N4'A C5'A C6'A -115.7(5) . . . . ?
C1 O2 C3 C11 166.4(5) . . . . ?
C1 O2 C3 C4 44.2(7) . . . . ?
C1 C9 C10 C5 -177.0(6) . . . . ?
C1 C9 C10 C4 -0.1(8) . . . . ?
C6A C7A C6'A C5'A 103.6(6) . . . . ?
C1' N2' C3' O17 178.5(5) . . . . ?
C1' N2' C3' N4' -1.4(6) . . . . ?
C1' C5' C6' C7 166.5(5) . . . . ?
C10 C9 C1 O2 -9.2(8) . . . . ?
C10 C9 C1 O20 170.4(6) . . . . ?
C5'A N4'A C3'A O40 175.4(5) . . . . ?
C5'A N4'A C3'A N2'A -4.2(6) . . . . ?
C7A C8A C9A C10A 1.4(8) . . . . ?
C7A C8A C9A C1A 175.2(5) . . . . ?
C7A C6A C5A C10A 0.2(9) . . . . ?
C10A C9A C1A O2A -6.8(9) . . . . ?
C10A C9A C1A O42 173.4(6) . . . . ?
C7 C8 C9 C1 179.2(5) . . . . ?
C7 C8 C9 C10 1.4(8) . . . . ?
C7 C6 C5 C10 2.8(9) . . . . ?
C1'A N2'A C3'A O40 -175.5(5) . . . . ?
C1'A N2'A C3'A N4'A 4.2(6) . . . . ?
C1'A C5'A C6'A C7A -179.3(5) . . . . ?
C1A O2A C3A C4A 45.8(7) . . . . ?
C1A O2A C3A C11A 170.4(5) . . . . ?
C1A C9A C10A C5A -179.5(6) . . . . ?
C1A C9A C10A C4A -2.1(8) . . . . ?
C3 O2 C1 O20 166.2(5) . . . . ?
C3 O2 C1 C9 -14.2(8) . . . . ?
C5A C6A C7A C8A -4.6(9) . . . . ?
C5A C6A C7A C6'A 171.9(5) . . . . ?
C5A C10A C4A C3A -151.3(5) . . . . ?
C5 C6 C7 C8 -0.6(8) . . . . ?
C5 C6 C7 C6' -179.0(5) . . . . ?
C5 C10 C4 C3 -153.2(6) . . . . ?
C5' N4' C3' O17 -179.0(6) . . . . ?
C5' N4' C3' N2' 0.8(6) . . . . ?
C11 C3 C4 C10 -167.6(5) . . . . ?
C6'A C5'A C1'A O39 -59.1(7) . . . . ?
C6'A C5'A C1'A N2'A 120.4(5) . . . . ?
C3A O2A C1A O42 163.7(5) . . . . ?
C3A O2A C1A C9A -16.2(8) . . . . ?
C4A C10A C5A C6A -172.2(5) . . . . ?
C4 C10 C5 C6 -179.6(5) . . . . ?
C11A C3A C4A C10A -171.5(5) . . . . ?
_shelx_res_file
;
bzl-82_collect.res created by SHELXL-2014/7
TITL bzl-82_collect_a.res in P2(1)
REM Old TITL BZL-82_collect in P2(1)
REM SHELXT solution in P2(1)
REM R1 0.089, Rweak 0.040, Alpha 0.002, Orientation as input
REM Flack x = 0.123 ( 0.129 ) from Parsons' quotients
REM Formula found by SHELXT: C7A N4 O12
CELL 1.54184 5.1422 35.611 7.3209 90 106.229 90
ZERR 2 0.0001 0.0008 0.0002 0 0.002 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O
UNIT 56 56 8 24
L.S. 4
PLAN 5
SIZE 0.1 0.02 0.03
BOND $H
LIST 4
MORE -1
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.097400 1.553400
FVAR 0.70598
O21 4 0.626284 0.589551 0.863590 11.00000 0.02241 0.02855 =
0.01981 0.00357 0.00142 -0.00618
AFIX 147
H21 2 0.495298 0.580063 0.786767 11.00000 -1.50000
AFIX 0
O17 4 0.664884 0.474318 0.564691 11.00000 0.02394 0.02340 =
0.02547 0.00268 0.00184 -0.00008
O2 4 1.389136 0.710058 0.636484 11.00000 0.02394 0.02940 =
0.01885 -0.00087 0.00716 -0.00508
O39 4 0.826010 0.458507 1.135102 11.00000 0.02031 0.02744 =
0.02181 0.00215 0.00018 -0.00116
O2A 4 -0.444963 0.290639 0.798353 11.00000 0.02599 0.02990 =
0.02337 0.00220 0.00256 -0.00711
O43 4 0.112820 0.420593 0.443512 11.00000 0.02562 0.03023 =
0.02125 0.00577 -0.00077 -0.00808
AFIX 147
H43 2 -0.001265 0.423694 0.341127 11.00000 -1.50000
AFIX 0
O20 4 1.165457 0.689898 0.351845 11.00000 0.03261 0.02984 =
0.01718 -0.00035 0.00570 -0.00207
O41 4 0.181542 0.365383 1.037666 11.00000 0.03057 0.03062 =
0.01735 0.00477 0.00223 -0.00742
AFIX 147
H41 2 0.109901 0.349067 1.086153 11.00000 -1.50000
AFIX 0
O40 4 0.236569 0.538260 0.731567 11.00000 0.02636 0.02166 =
0.02110 0.00379 0.00065 0.00156
O18 4 0.066219 0.548782 0.137539 11.00000 0.02351 0.02852 =
0.02489 -0.00114 -0.00424 -0.00204
O19 4 0.759111 0.644810 0.305263 11.00000 0.02932 0.02977 =
0.01474 0.00345 0.00163 -0.00133
AFIX 147
H19 2 0.862920 0.659369 0.274366 11.00000 -1.50000
AFIX 0
O42 4 -0.128818 0.309268 1.050593 11.00000 0.03524 0.03289 =
0.02203 0.00442 0.00254 -0.00647
N2' 3 0.322084 0.504118 0.335489 11.00000 0.01306 0.02542 =
0.02461 -0.00182 0.00548 -0.00438
AFIX 43
H2' 2 0.211847 0.485484 0.306325 11.00000 -1.20000
AFIX 0
N2'A 3 0.578347 0.506107 0.954729 11.00000 0.02190 0.01900 =
0.01725 0.00120 -0.00018 -0.00289
AFIX 43
H2'A 2 0.695652 0.523900 0.984836 11.00000 -1.20000
AFIX 0
N4'A 3 0.189446 0.477436 0.824746 11.00000 0.01493 0.02177 =
0.02287 0.00052 0.00335 -0.00073
AFIX 43
H4'A 2 0.023409 0.473856 0.761207 11.00000 -1.20000
AFIX 0
N4' 3 0.690163 0.535992 0.474416 11.00000 0.01649 0.01984 =
0.02554 -0.00268 0.00025 -0.00093
AFIX 43
H4' 2 0.848703 0.541359 0.546600 11.00000 -1.20000
AFIX 0
C3' 1 0.574293 0.502297 0.470244 11.00000 0.01803 0.02510 =
0.01847 -0.00321 0.00612 0.00020
C8 1 0.827856 0.641858 0.496123 11.00000 0.01809 0.02517 =
0.01581 -0.00152 0.00432 0.00521
C9 1 1.048349 0.662519 0.612055 11.00000 0.01968 0.02264 =
0.01973 0.00170 0.00450 0.00109
C8A 1 0.060712 0.366630 0.848617 11.00000 0.01329 0.02433 =
0.02026 -0.00027 0.00542 0.00346
C6 1 0.757412 0.612101 0.771576 11.00000 0.02303 0.02063 =
0.02163 0.00385 0.00526 0.00153
C9A 1 -0.156741 0.341954 0.764016 11.00000 0.01711 0.02264 =
0.02073 0.00109 0.00455 -0.00044
C3'A 1 0.319434 0.509762 0.825386 11.00000 0.02184 0.02103 =
0.01683 -0.00279 0.00706 0.00075
C1 1 1.200911 0.687950 0.524750 11.00000 0.02136 0.02292 =
0.02061 -0.00064 0.00350 0.00213
C6A 1 0.024370 0.394589 0.545480 11.00000 0.01945 0.01919 =
0.02458 0.00104 0.00439 -0.00112
C1' 1 0.270548 0.538833 0.255393 11.00000 0.01686 0.02201 =
0.02445 -0.00486 0.00579 -0.00042
C10 1 1.120035 0.656839 0.810029 11.00000 0.02126 0.02035 =
0.01922 -0.00079 0.00223 0.00101
C5'A 1 0.356472 0.448932 0.942061 11.00000 0.01233 0.02191 =
0.02272 0.00254 0.00613 -0.00184
AFIX 13
H5'A 2 0.277563 0.440918 1.043051 11.00000 -1.20000
AFIX 0
C7A 1 0.157224 0.392235 0.739161 11.00000 0.01941 0.02016 =
0.02282 -0.00282 0.00262 0.00120
C10A 1 -0.270247 0.343146 0.566118 11.00000 0.01512 0.02668 =
0.02405 -0.00445 0.00276 0.00269
C7 1 0.679234 0.617022 0.573099 11.00000 0.01800 0.01976 =
0.01982 -0.00007 0.00523 0.00258
C1'A 1 0.617716 0.470624 1.025567 11.00000 0.01675 0.02171 =
0.01655 -0.00029 0.00646 0.00048
C1A 1 -0.239463 0.313388 0.879977 11.00000 0.01936 0.02424 =
0.02538 -0.00562 0.00209 -0.00149
C3 1 1.396894 0.715081 0.838464 11.00000 0.01717 0.02966 =
0.02088 -0.00257 0.00817 -0.00024
AFIX 13
H3 2 1.251845 0.732252 0.847055 11.00000 -1.20000
AFIX 0
C5A 1 -0.188360 0.370130 0.458811 11.00000 0.02322 0.02364 =
0.01693 0.00070 -0.00006 -0.00118
AFIX 43
H5A 2 -0.273961 0.372112 0.329261 11.00000 -1.20000
AFIX 0
C5 1 0.981613 0.631593 0.887474 11.00000 0.02166 0.02375 =
0.01609 0.00176 0.00237 0.00018
AFIX 43
H5 2 1.035762 0.627219 1.017900 11.00000 -1.20000
AFIX 0
C5' 1 0.519414 0.562614 0.343800 11.00000 0.01944 0.02199 =
0.02163 -0.00094 0.00104 -0.00145
AFIX 13
H5' 2 0.606086 0.570573 0.246780 11.00000 -1.20000
AFIX 0
C6' 1 0.436974 0.597129 0.443422 11.00000 0.02249 0.02243 =
0.01914 -0.00121 0.00156 0.00005
AFIX 23
H6'A 2 0.337642 0.614625 0.347598 11.00000 -1.20000
H6'B 2 0.317363 0.589048 0.517425 11.00000 -1.20000
AFIX 0
C11 1 1.668557 0.733174 0.929627 11.00000 0.02690 0.02549 =
0.02586 -0.00619 0.00802 -0.00385
AFIX 137
H11A 2 1.810653 0.717191 0.913162 11.00000 -1.50000
H11B 2 1.689641 0.736782 1.062937 11.00000 -1.50000
H11C 2 1.677683 0.757024 0.870603 11.00000 -1.50000
AFIX 0
C6'A 1 0.408407 0.414854 0.828380 11.00000 0.01677 0.02212 =
0.02042 -0.00077 0.00398 0.00041
AFIX 23
H6'C 2 0.484938 0.423535 0.728911 11.00000 -1.20000
H6'D 2 0.541101 0.398685 0.912404 11.00000 -1.20000
AFIX 0
C3A 1 -0.628182 0.300577 0.611926 11.00000 0.02097 0.02372 =
0.02635 -0.00210 0.00615 -0.00135
AFIX 13
H3A 2 -0.743794 0.321368 0.629385 11.00000 -1.20000
AFIX 0
C4A 1 -0.472426 0.313083 0.477959 11.00000 0.01997 0.02558 =
0.02345 -0.00173 0.00390 -0.00132
AFIX 23
H4AA 2 -0.597163 0.322695 0.362410 11.00000 -1.20000
H4AB 2 -0.378166 0.291752 0.444042 11.00000 -1.20000
AFIX 0
C4 1 1.361553 0.678080 0.928130 11.00000 0.02326 0.02399 =
0.01771 -0.00198 0.00378 -0.00087
AFIX 23
H4A 2 1.523192 0.662987 0.943065 11.00000 -1.20000
H4B 2 1.339350 0.682544 1.053617 11.00000 -1.20000
AFIX 0
C11A 1 -0.804465 0.266733 0.544512 11.00000 0.01987 0.03040 =
0.02959 -0.00298 0.00606 -0.00189
AFIX 137
H11D 2 -0.692341 0.245213 0.543711 11.00000 -1.50000
H11E 2 -0.918721 0.271199 0.418228 11.00000 -1.50000
H11F 2 -0.914709 0.262210 0.628623 11.00000 -1.50000
AFIX 0
HKLF 4
REM bzl-82_collect_a.res in P2(1)
REM R1 = 0.0594 for 4399 Fo > 4sig(Fo) and 0.0667 for all 4938 data
REM 403 parameters refined using 1 restraints
END
WGHT 0.0974 1.5534
REM Highest difference peak 0.464, deepest hole -0.342, 1-sigma level 0.089
Q1 1 0.3023 0.4212 0.4581 11.00000 0.05 0.46
Q2 1 0.8973 0.5611 0.3648 11.00000 0.05 0.45
Q3 1 0.5132 0.4201 0.4590 11.00000 0.05 0.45
Q4 1 1.0345 0.5911 0.8642 11.00000 0.05 0.44
Q5 1 1.0950 0.5373 0.4702 11.00000 0.05 0.43
;
_shelx_res_checksum 98834
_shelx_hkl_file
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5 -3 -5 6.62 2.32
5 -3 -5 5.26 4.23
5 -3 -4 68.31 3.33
5 -3 -4 74.11 6.13
5 -3 -3 26.68 3.88
5 -3 -3 29.22 6.22
5 -3 -2 92.15 6.53
5 -3 -2 108.82 7.61
5 -3 -1 23.95 7.13
5 -3 -1 15.90 5.85
5 -3 0 82.78 7.89
5 -3 1 22.94 5.88
5 -3 1 7.00 7.03
5 -3 2 -6.81 4.79
5 -3 3 14.98 3.64
5 -2 -7 9.29 1.69
5 -2 -6 6.56 2.22
5 -2 -5 37.17 2.84
5 -2 -5 34.01 4.41
5 -2 -4 100.24 3.96
5 -2 -4 125.44 6.86
5 -2 -3 53.40 5.58
5 -2 -3 40.19 6.25
5 -2 -2 141.99 7.65
5 -2 -2 158.29 8.96
5 -2 -1 145.12 8.91
5 -2 -1 170.99 9.65
5 -2 0 57.76 7.44
5 -2 1 122.58 9.17
5 -2 1 137.28 7.76
5 -2 2 6.58 5.00
5 -2 3 9.83 3.42
5 -1 -7 56.20 2.46
5 -1 -6 29.52 2.71
5 -1 -5 41.59 2.84
5 -1 -5 38.84 4.19
5 -1 -4 15.77 2.15
5 -1 -4 19.79 4.53
5 -1 -3 83.40 6.13
5 -1 -3 69.87 6.72
5 -1 -2 77.11 6.17
5 -1 -2 92.43 7.77
5 -1 -1 47.88 6.40
5 -1 -1 51.44 7.47
5 -1 0 7.85 6.82
5 -1 1 96.13 8.51
5 -1 1 112.86 7.12
5 -1 2 -6.88 5.41
5 -1 3 60.63 4.38
5 0 -7 13.06 1.69
5 0 -6 110.09 4.22
5 0 -5 7.84 2.33
5 0 -5 14.68 3.51
5 0 -4 29.64 2.51
5 0 -4 49.20 4.78
5 0 -3 24.41 5.08
5 0 -3 13.88 5.18
5 0 -2 368.63 12.91
5 0 -2 410.44 14.22
5 0 -1 44.32 6.41
5 0 -1 57.78 7.94
5 0 0 125.23 9.10
5 0 1 21.42 5.74
5 0 1 1.12 6.52
5 0 2 88.56 6.27
5 0 3 24.03 3.89
5 1 -7 58.71 2.47
5 1 -6 28.26 2.57
5 1 -5 30.06 2.79
5 1 -4 7.65 2.09
5 1 -4 18.80 4.00
5 1 -3 82.20 6.17
5 1 -3 66.44 5.88
5 1 -2 62.27 5.60
5 1 -2 83.29 7.58
5 1 -1 40.07 6.48
5 1 -1 48.67 7.42
5 1 0 4.92 6.39
5 1 1 97.37 8.40
5 1 1 112.15 7.35
5 1 3 58.85 4.56
5 2 -7 8.62 1.47
5 2 -6 4.60 2.04
5 2 -5 24.84 2.56
5 2 -4 92.06 3.66
5 2 -3 47.67 5.59
5 2 -3 38.91 4.94
5 2 -2 124.44 6.90
5 2 -2 114.00 6.48
5 2 -1 143.50 8.52
5 2 -1 167.35 9.69
5 2 0 44.71 7.35
5 2 1 122.86 9.00
5 2 1 141.20 8.19
5 2 2 24.55 4.48
5 2 3 8.72 3.43
5 3 -7 24.40 1.69
5 3 -6 19.19 2.25
5 3 -5 -1.72 2.14
5 3 -3 33.06 4.13
5 3 -3 36.22 5.37
5 3 -2 78.82 5.99
5 3 -2 92.49 7.79
5 3 -1 5.00 5.28
5 3 -1 6.01 6.86
5 3 0 74.46 7.93
5 3 1 -1.46 6.47
5 3 1 12.22 6.17
5 3 2 22.46 4.23
5 3 3 14.76 3.69
5 4 -7 20.57 1.55
5 4 -6 70.00 3.10
5 4 -5 1.70 2.06
5 4 -4 38.23 3.89
5 4 -3 46.95 4.62
5 4 -3 57.20 6.00
5 4 -2 85.11 6.33
5 4 -2 93.52 8.22
5 4 -1 25.47 5.80
5 4 -1 24.37 7.00
5 4 0 139.81 8.86
5 4 1 -0.84 6.88
5 4 1 8.79 5.70
5 4 2 54.90 4.63
5 4 3 6.69 3.47
5 5 -7 22.79 1.54
5 5 -6 35.41 2.39
5 5 -5 60.26 2.97
5 5 -4 129.19 5.98
5 5 -3 137.73 6.71
5 5 -3 165.39 8.19
5 5 -2 185.05 8.50
5 5 -2 224.70 10.27
5 5 -1 204.02 9.85
5 5 -1 218.03 10.86
5 5 0 159.73 9.16
5 5 1 24.38 6.45
5 5 1 36.49 6.29
5 5 2 52.58 4.70
5 5 3 16.47 3.56
5 6 -7 22.94 1.50
5 6 -6 72.23 3.05
5 6 -5 28.22 2.29
5 6 -5 22.59 3.35
5 6 -4 6.78 3.64
5 6 -3 144.90 6.92
5 6 -3 162.21 8.14
5 6 -2 285.49 11.08
5 6 -2 363.79 12.85
5 6 -1 171.03 9.03
5 6 -1 189.18 10.18
5 6 0 14.87 5.96
5 6 1 9.50 6.68
5 6 1 8.95 5.72
5 6 2 102.33 5.61
5 6 3 20.16 3.50
5 7 -7 107.04 3.24
5 7 -6 31.05 2.07
5 7 -5 59.08 2.80
5 7 -5 52.44 4.08
5 7 -4 77.59 5.05
5 7 -3 92.28 5.82
5 7 -3 103.91 6.96
5 7 -2 126.66 7.45
5 7 -2 134.18 8.70
5 7 -1 241.13 10.39
5 7 -1 248.52 11.52
5 7 0 40.68 6.64
5 7 1 50.33 6.63
5 7 1 43.94 6.46
5 7 2 17.89 3.90
5 7 3 88.34 4.66
5 8 -7 21.24 1.31
5 8 -6 47.35 2.31
5 8 -5 32.88 2.14
5 8 -5 24.09 3.67
5 8 -4 37.32 4.43
5 8 -3 101.50 5.92
5 8 -3 94.52 6.64
5 8 -2 126.43 7.51
5 8 -2 136.22 8.36
5 8 -1 41.85 7.38
5 8 -1 55.09 6.01
5 8 0 99.81 8.01
5 8 1 73.97 6.96
5 8 1 54.04 6.57
5 8 2 144.75 6.42
5 8 3 44.67 3.74
5 9 -7 26.73 1.44
5 9 -6 33.58 1.96
5 9 -6 14.47 2.64
5 9 -5 94.14 3.40
5 9 -5 90.45 5.06
5 9 -4 46.69 4.74
5 9 -3 187.88 8.03
5 9 -3 192.24 8.69
5 9 -2 154.55 8.02
5 9 -2 156.41 8.73
5 9 -1 51.25 7.41
5 9 -1 71.46 6.36
5 9 0 90.43 7.81
5 9 1 59.84 6.79
5 9 1 46.67 6.28
5 9 2 69.40 4.86
5 9 3 8.29 2.86
5 10 -7 26.53 1.39
5 10 -6 77.30 2.72
5 10 -6 53.65 3.56
5 10 -5 59.66 2.56
5 10 -5 49.73 4.31
5 10 -4 69.12 5.27
5 10 -3 178.67 7.81
5 10 -3 163.37 7.99
5 10 -2 139.84 7.66
5 10 -2 128.72 8.22
5 10 -1 57.93 6.94
5 10 -1 80.69 6.53
5 10 -1 62.95 7.34
5 10 0 206.46 10.20
5 10 1 86.81 7.22
5 10 1 68.07 6.47
5 10 2 66.75 5.80
5 10 2 71.55 4.71
5 10 3 7.49 2.56
5 11 -6 31.07 1.78
5 11 -6 14.49 2.71
5 11 -5 60.23 2.56
5 11 -5 52.65 4.39
5 11 -4 40.29 4.74
5 11 -3 132.09 6.86
5 11 -3 113.53 6.97
5 11 -2 99.48 6.97
5 11 -2 88.18 7.13
5 11 -1 40.29 6.91
5 11 -1 62.39 6.40
5 11 -1 55.25 6.78
5 11 0 165.01 10.08
5 11 1 28.72 6.43
5 11 1 9.79 5.16
5 11 2 100.61 6.43
5 11 2 98.85 5.15
5 11 3 1.00 2.27
5 12 -6 35.57 1.93
5 12 -6 26.43 2.90
5 12 -5 37.44 2.05
5 12 -5 32.29 4.00
5 12 -4 36.47 4.82
5 12 -3 61.65 5.46
5 12 -3 52.41 5.49
5 12 -2 5.83 5.19
5 12 -2 12.74 5.56
5 12 -1 68.33 7.34
5 12 -1 79.72 6.59
5 12 -1 78.08 6.97
5 12 0 59.95 7.34
5 12 1 72.50 6.67
5 12 1 54.12 5.91
5 12 2 84.69 5.87
5 12 2 88.42 4.69
5 13 -6 6.53 1.36
5 13 -6 3.54 2.40
5 13 -5 17.32 1.74
5 13 -5 13.74 3.68
5 13 -4 8.90 4.23
5 13 -3 49.41 5.25
5 13 -3 35.83 4.95
5 13 -2 93.94 6.88
5 13 -2 89.32 6.56
5 13 -1 129.74 8.52
5 13 -1 147.79 8.33
5 13 -1 136.00 8.14
5 13 0 28.86 5.92
5 13 1 36.01 6.63
5 13 1 19.11 5.04
5 13 2 -0.53 3.99
5 13 2 2.71 2.93
5 14 -6 29.05 1.65
5 14 -6 22.49 2.77
5 14 -5 22.97 1.79
5 14 -5 18.91 3.76
5 14 -4 30.56 4.65
5 14 -3 9.41 4.40
5 14 -3 21.68 5.05
5 14 -2 5.75 4.99
5 14 -2 15.79 5.86
5 14 -1 52.44 7.16
5 14 -1 51.41 6.37
5 14 -1 49.82 6.34
5 14 0 21.91 5.55
5 14 1 71.62 7.16
5 14 1 45.02 5.36
5 14 2 111.20 5.84
5 14 2 96.00 4.61
5 15 -6 48.24 1.95
5 15 -6 46.14 3.18
5 15 -5 28.32 1.82
5 15 -5 25.84 3.84
5 15 -4 130.84 6.69
5 15 -3 12.79 4.32
5 15 -3 26.22 5.05
5 15 -2 19.71 5.15
5 15 -2 26.42 5.86
5 15 -1 40.30 6.92
5 15 -1 41.11 5.88
5 15 -1 37.23 5.75
5 15 0 336.06 12.14
5 15 1 24.20 5.68
5 15 1 7.67 4.55
5 15 2 60.03 4.50
5 15 2 49.08 3.38
5 16 -6 30.54 1.47
5 16 -6 29.82 2.70
5 16 -5 16.39 1.48
5 16 -5 14.07 3.47
5 16 -4 122.15 6.24
5 16 -3 5.34 3.90
5 16 -3 18.95 4.89
5 16 -2 287.78 11.17
5 16 -2 304.85 10.81
5 16 -1 48.65 5.12
5 16 -1 53.42 5.84
5 16 0 85.23 6.11
5 16 1 26.94 4.47
5 16 1 44.68 6.06
5 16 2 23.37 3.45
5 16 2 18.75 2.50
5 17 -6 9.39 2.21
5 17 -5 81.42 2.74
5 17 -5 102.69 4.95
5 17 -4 65.78 5.16
5 17 -3 9.59 3.84
5 17 -3 26.27 5.03
5 17 -2 25.72 4.59
5 17 -2 27.71 6.01
5 17 -1 38.24 4.65
5 17 -1 44.06 5.57
5 17 0 166.97 7.69
5 17 1 62.76 6.06
5 17 1 33.59 4.51
5 17 2 5.54 3.00
5 18 -6 31.11 2.33
5 18 -5 16.12 3.38
5 18 -4 58.20 4.75
5 18 -3 13.26 3.75
5 18 -3 30.85 4.91
5 18 -2 98.01 6.82
5 18 -2 107.70 6.27
5 18 -1 27.20 4.70
5 18 -1 25.93 4.13
5 18 0 47.62 4.88
5 18 1 82.94 6.07
5 18 1 52.53 4.62
5 18 2 7.04 2.70
5 19 -5 25.64 3.24
5 19 -4 42.61 4.26
5 19 -3 1.40 3.29
5 19 -3 7.84 3.80
5 19 -2 23.59 4.27
5 19 -2 31.85 5.82
5 19 -1 6.70 4.20
5 19 -1 5.44 4.48
5 19 0 86.02 5.40
5 19 1 25.76 4.67
5 19 1 11.56 3.57
5 19 2 20.53 2.62
5 20 -5 17.53 3.09
5 20 -4 24.92 3.21
5 20 -4 47.57 4.15
5 20 -3 29.77 4.18
5 20 -3 31.95 3.64
5 20 -2 122.48 7.07
5 20 -2 116.24 6.07
5 20 -1 58.22 5.16
5 20 0 13.24 3.94
5 20 1 99.75 5.68
5 20 1 71.47 4.51
5 21 -5 47.83 3.39
5 21 -4 12.10 3.05
5 21 -4 21.14 3.65
5 21 -3 10.81 3.09
5 21 -3 15.05 3.73
5 21 -2 30.76 5.26
5 21 -2 25.32 3.91
5 21 -1 25.51 4.27
5 21 0 9.86 3.51
5 21 1 65.28 4.25
5 21 1 51.59 3.79
5 22 -5 2.83 2.22
5 22 -4 7.15 2.81
5 22 -4 17.86 3.51
5 22 -3 12.31 3.60
5 22 -3 34.55 4.49
5 22 -2 102.31 5.39
5 22 -1 31.93 4.18
5 22 0 40.39 3.66
5 22 1 6.25 2.63
5 22 1 -1.63 2.44
5 23 -5 24.14 2.43
5 23 -4 9.07 2.39
5 23 -4 19.85 3.29
5 23 -2 96.95 5.08
5 23 -1 22.77 3.71
5 23 0 19.98 3.30
5 23 1 24.86 2.50
5 24 -2 9.28 2.82
5 24 -1 49.42 3.94
5 25 -2 109.07 4.67
5 25 -1 98.60 4.60
5 26 -4 24.81 2.37
5 26 -3 12.35 3.01
5 26 -2 27.76 2.61
5 26 -1 25.51 2.78
5 27 -1 35.82 2.66
6 -15 -3 5.12 2.10
6 -15 -2 1.91 2.16
6 -14 -3 13.39 2.40
6 -14 -2 10.12 2.65
6 -14 -1 21.51 2.61
6 -13 -3 22.57 2.74
6 -13 -2 4.74 2.55
6 -13 -2 3.14 2.79
6 -13 -1 11.50 2.74
6 -13 -1 5.88 2.50
6 -12 -3 3.18 2.64
6 -12 -2 52.25 3.61
6 -12 -2 54.46 3.82
6 -12 -1 40.17 3.39
6 -12 -1 38.20 3.30
6 -11 -4 12.66 2.36
6 -11 -3 3.26 2.68
6 -11 -2 16.65 3.11
6 -11 -2 7.95 3.27
6 -11 -1 30.43 3.12
6 -11 -1 4.34 2.86
6 -10 -4 3.93 1.90
6 -10 -3 25.01 3.12
6 -10 -2 64.99 3.71
6 -10 -2 30.53 3.80
6 -10 -1 51.04 3.44
6 -10 -1 12.80 3.11
6 -10 0 31.96 2.63
6 -9 -4 25.53 2.25
6 -9 -3 12.07 2.98
6 -9 -2 65.63 3.74
6 -9 -2 30.25 3.71
6 -9 -1 43.49 3.44
6 -9 -1 -1.78 3.08
6 -8 -4 3.13 1.96
6 -8 -3 20.22 3.14
6 -8 -2 72.18 4.07
6 -8 -2 43.59 4.00
6 -8 -1 45.06 3.57
6 -8 -1 10.33 3.21
6 -7 -4 11.00 1.98
6 -7 -3 40.75 3.32
6 -7 -2 90.88 4.61
6 -7 -2 76.73 4.58
6 -7 -1 42.30 3.70
6 -7 -1 12.87 3.19
6 -6 -3 39.66 3.19
6 -6 -2 27.91 3.71
6 -6 -2 7.00 3.31
6 -6 -1 29.96 3.67
6 -6 -1 7.84 2.88
6 -6 0 15.28 2.61
6 -5 -3 81.32 3.70
6 -5 -3 63.33 3.60
6 -5 -2 78.54 4.63
6 -5 -2 63.74 4.18
6 -5 -1 50.11 4.17
6 -5 -1 25.30 3.16
6 -5 0 100.08 4.36
6 -4 -3 104.02 4.26
6 -4 -2 69.28 4.76
6 -4 -2 57.60 3.70
6 -4 -1 9.00 3.97
6 -4 -1 6.83 2.56
6 -4 0 27.31 2.95
6 -3 -3 34.34 3.08
6 -3 -2 1.67 3.96
6 -3 -1 11.38 4.30
6 -3 0 36.36 3.20
6 -2 -3 6.05 2.74
6 -2 -2 77.55 5.30
6 -2 0 8.14 2.75
6 -1 -3 68.03 3.75
6 -1 -2 15.30 4.43
6 -1 0 19.75 2.96
6 0 -3 20.12 3.21
6 0 -2 145.79 6.87
6 0 -1 75.12 5.62
6 0 0 20.78 2.97
6 1 -3 62.86 3.82
6 1 -2 8.94 5.03
6 1 0 20.30 3.01
6 2 -2 85.10 5.74
6 2 0 7.07 2.66
6 3 -3 8.41 3.04
6 3 0 35.69 2.98
6 4 -2 43.66 4.77
6 5 -2 57.06 4.80
6 5 -1 44.92 4.15
6 6 -2 18.47 3.58
6 6 -1 33.14 3.77
6 7 -2 84.36 4.60
6 7 -1 29.77 3.54
6 8 -2 57.36 3.86
6 8 -1 26.86 3.34
6 9 -2 41.80 3.44
6 9 -1 10.24 3.00
6 10 -2 38.97 3.22
6 10 -1 24.01 2.98
6 11 -2 13.42 2.60
6 11 -1 18.06 2.75
6 12 -2 62.99 3.37
6 12 -1 47.34 3.15
6 13 -2 6.50 2.05
6 13 -1 17.04 2.34
0 0 0 0.00 0.00
TITL BZL-82_collect in P2(1)
REM P2(1) (#4 in standard setting)
CELL 1.54184 5.142223 35.611026 7.320867 90.0000 106.2288 90.0000
ZERR 1.00 0.000116 0.000827 0.000165 0.0000 0.0024 0.0000
LATT -1
SYMM -x, y+1/2,-z
SFAC C H N O
UNIT 1.00 1.00 1.00 1.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 18759
_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 5.441
_oxdiff_exptl_absorpt_empirical_full_min 0.258
_chemical_compound_source insect