# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2020
#######################################################################
#
# 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_20181222_mdl_zhp_ch9_67
_database_code_depnum_ccdc_archive 'CCDC 1938292'
loop_
_audit_author_name
_audit_author_address
'Dong-Liang Mo'
;Guangxi Normal University
China
;
_audit_update_record
;
2019-07-04 deposited with the CCDC. 2020-09-25 downloaded from the CCDC.
;
_audit_creation_date 2019-07-03
_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 ?
_chemical_name_systematic ?
_chemical_formula_moiety '0.57(C18 H18 N2 O3)'
_chemical_formula_sum 'C11 H10 N O'
_chemical_formula_weight 172.20
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_H-M_alt 'P b c a'
_space_group_name_Hall '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
_cell_length_a 15.014(2)
_cell_length_b 10.0228(11)
_cell_length_c 21.573(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3246.5(9)
_cell_formula_units_Z 14
_cell_measurement_reflns_used 1041
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 21.1890
_cell_measurement_theta_min 3.8650
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.080
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.43184
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour white
_exptl_crystal_density_diffrn 1.233
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1274
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0588
_diffrn_reflns_av_unetI/netI 0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 11068
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.946
_diffrn_reflns_theta_min 3.306
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.884
_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 -12.00 57.00 1.00 10.00 -- 17.61 77.00 150.00 69
2 \w -86.00 23.00 1.00 10.00 -- -19.80 -19.00 0.00 109
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0192021000
_diffrn_orient_matrix_UB_12 0.0030643000
_diffrn_orient_matrix_UB_13 -0.0300338000
_diffrn_orient_matrix_UB_21 -0.0419370000
_diffrn_orient_matrix_UB_22 0.0181526000
_diffrn_orient_matrix_UB_23 -0.0125614000
_diffrn_orient_matrix_UB_31 0.0103373000
_diffrn_orient_matrix_UB_32 0.0682769000
_diffrn_orient_matrix_UB_33 0.0046471000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 1287
_reflns_number_total 3794
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 26.32
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.384
_refine_diff_density_min -0.239
_refine_diff_density_rms 0.048
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.018
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 211
_refine_ls_number_reflns 3794
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.2084
_refine_ls_R_factor_gt 0.0871
_refine_ls_restrained_S_all 1.018
_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^)+(0.1206P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2286
_refine_ls_wR_factor_ref 0.3103
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
N2(H2), C12(H12), C6(H6), C3(H3), C10(H10), C9(H9), C4(H4), C5(H5), C11(H11)
2.b Idealised Me refined as rotating group:
C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_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 0.24312(19) 0.4715(2) 0.07639(18) 0.0891(12) Uani 1 1 d . . . . .
O1 O 0.4073(2) 0.2254(3) 0.12061(15) 0.0813(10) Uani 1 1 d . . . . .
N2 N 0.2418(2) 0.2490(3) 0.07644(19) 0.0705(11) Uani 1 1 d . . . . .
H2 H 0.2701 0.1756 0.0825 0.085 Uiso 1 1 calc R . . . .
C17 C 0.2800(3) 0.3651(4) 0.0882(2) 0.0621(12) Uani 1 1 d . . . . .
O3 O 0.1554(2) 0.2479(3) 0.0541(2) 0.0835(11) Uani 1 1 d . . . . .
N1 N 0.3708(3) 0.1665(4) 0.17145(19) 0.0765(11) Uani 1 1 d . . . . .
C1 C 0.4038(3) 0.0426(4) 0.1783(2) 0.0768(14) Uani 1 1 d . . . . .
C15 C 0.3735(3) 0.3636(3) 0.1153(2) 0.0643(12) Uani 1 1 d . . . . .
C8 C 0.4214(3) -0.1587(4) 0.2273(2) 0.0727(13) Uani 1 1 d . . . . .
C7 C 0.4806(3) -0.1582(4) 0.1744(2) 0.0743(14) Uani 1 1 d . . . . .
C13 C 0.3742(4) -0.0348(5) 0.2306(3) 0.0780(14) Uani 1 1 d . . . . .
C12 C 0.3153(4) -0.0120(5) 0.2775(3) 0.0918(16) Uani 1 1 d . . . . .
H12 H 0.2849 0.0687 0.2796 0.110 Uiso 1 1 calc R . . . .
C6 C 0.5390(4) -0.2530(5) 0.1529(3) 0.0875(16) Uani 1 1 d . . . . .
H6 H 0.5464 -0.3330 0.1741 0.105 Uiso 1 1 calc R . . . .
C14 C 0.3765(3) 0.4399(4) 0.1755(2) 0.0834(15) Uani 1 1 d . . . . .
H14A H 0.3369 0.3991 0.2048 0.125 Uiso 1 1 calc GR . . . .
H14B H 0.3585 0.5305 0.1683 0.125 Uiso 1 1 calc GR . . . .
H14C H 0.4361 0.4387 0.1916 0.125 Uiso 1 1 calc GR . . . .
C2 C 0.4686(3) -0.0336(5) 0.1436(2) 0.0773(14) Uani 1 1 d . . . . .
C16 C 0.4361(3) 0.4216(4) 0.0684(2) 0.0845(15) Uani 1 1 d . . . . .
H16A H 0.4948 0.4275 0.0859 0.127 Uiso 1 1 calc GR . . . .
H16B H 0.4161 0.5092 0.0568 0.127 Uiso 1 1 calc GR . . . .
H16C H 0.4376 0.3654 0.0323 0.127 Uiso 1 1 calc GR . . . .
C3 C 0.5168(4) -0.0119(5) 0.0918(3) 0.0916(16) Uani 1 1 d . . . . .
H3 H 0.5101 0.0693 0.0715 0.110 Uiso 1 1 calc R . . . .
C10 C 0.3459(5) -0.2256(7) 0.3186(3) 0.107(2) Uani 1 1 d . . . . .
H10 H 0.3357 -0.2897 0.3490 0.129 Uiso 1 1 calc R . . . .
C18 C 0.1583(4) 0.2438(6) -0.0107(3) 0.123(2) Uani 1 1 d . . . . .
H18A H 0.0987 0.2401 -0.0268 0.184 Uiso 1 1 calc GR . . . .
H18B H 0.1906 0.1661 -0.0238 0.184 Uiso 1 1 calc GR . . . .
H18C H 0.1875 0.3224 -0.0260 0.184 Uiso 1 1 calc GR . . . .
C9 C 0.4059(4) -0.2515(5) 0.2720(3) 0.0885(16) Uani 1 1 d . . . . .
H9 H 0.4360 -0.3327 0.2711 0.106 Uiso 1 1 calc R . . . .
C4 C 0.5755(4) -0.1037(6) 0.0673(3) 0.1001(17) Uani 1 1 d . . . . .
H4 H 0.6069 -0.0858 0.0310 0.120 Uiso 1 1 calc R . . . .
C5 C 0.5865(4) -0.2277(6) 0.0996(3) 0.1056(19) Uani 1 1 d . . . . .
H5 H 0.6259 -0.2914 0.0844 0.127 Uiso 1 1 calc R . . . .
C11 C 0.3010(5) -0.1071(8) 0.3211(3) 0.117(2) Uani 1 1 d . . . . .
H11 H 0.2604 -0.0916 0.3529 0.140 Uiso 1 1 calc R . . . .
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 0.077(2) 0.0371(15) 0.153(3) 0.0018(16) -0.017(2) 0.0073(14)
O1 0.090(2) 0.0646(19) 0.089(2) 0.0160(16) -0.012(2) -0.0052(16)
N2 0.065(2) 0.0397(17) 0.107(3) -0.0008(17) -0.018(2) 0.0034(15)
C17 0.065(3) 0.041(2) 0.080(3) -0.0014(18) 0.006(2) -0.0005(19)
O3 0.063(2) 0.0577(18) 0.129(3) -0.0031(18) -0.008(2) -0.0025(13)
N1 0.075(3) 0.078(3) 0.076(3) -0.004(2) -0.002(2) -0.002(2)
C1 0.076(3) 0.056(3) 0.097(4) -0.013(3) -0.027(3) 0.003(2)
C15 0.076(3) 0.035(2) 0.082(3) 0.0002(19) -0.006(2) 0.0048(19)
C8 0.080(3) 0.061(3) 0.078(3) 0.001(2) -0.029(3) -0.007(2)
C7 0.084(3) 0.045(2) 0.094(4) 0.004(2) -0.041(3) 0.000(2)
C13 0.086(3) 0.063(3) 0.085(4) 0.009(3) -0.029(3) -0.010(3)
C12 0.082(4) 0.092(4) 0.101(4) -0.021(3) -0.016(3) 0.001(3)
C6 0.103(4) 0.066(3) 0.094(4) 0.007(3) -0.030(3) 0.006(3)
C14 0.110(4) 0.060(3) 0.080(3) -0.013(2) -0.013(3) 0.003(2)
C2 0.079(3) 0.081(3) 0.072(3) 0.008(3) -0.017(3) -0.019(3)
C16 0.076(3) 0.064(3) 0.113(4) 0.007(3) 0.002(3) 0.003(2)
C3 0.093(4) 0.075(3) 0.107(4) -0.008(3) -0.013(4) 0.011(3)
C10 0.127(6) 0.099(5) 0.095(5) 0.014(4) -0.021(4) -0.024(4)
C18 0.118(5) 0.116(5) 0.133(6) 0.028(4) -0.049(5) -0.024(4)
C9 0.108(5) 0.072(3) 0.085(4) 0.011(3) -0.027(4) -0.013(3)
C4 0.096(4) 0.109(4) 0.095(4) 0.002(3) -0.004(3) -0.015(3)
C5 0.110(5) 0.092(4) 0.115(5) -0.021(4) -0.024(4) 0.011(3)
C11 0.124(5) 0.132(6) 0.093(5) 0.019(4) -0.009(4) -0.034(5)
_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 C17 1.228(4) . ?
O1 N1 1.361(4) . ?
O1 C15 1.480(4) . ?
N2 C17 1.322(4) . ?
N2 O3 1.383(4) . ?
C17 C15 1.521(6) . ?
O3 C18 1.401(7) . ?
N1 C1 1.345(6) . ?
C1 C13 1.438(7) . ?
C1 C2 1.446(7) . ?
C15 C14 1.507(6) . ?
C15 C16 1.499(6) . ?
C8 C7 1.446(7) . ?
C8 C13 1.432(6) . ?
C8 C9 1.360(7) . ?
C7 C6 1.374(7) . ?
C7 C2 1.426(6) . ?
C13 C12 1.364(7) . ?
C12 C11 1.357(7) . ?
C6 C5 1.377(8) . ?
C2 C3 1.349(7) . ?
C3 C4 1.380(7) . ?
C10 C9 1.374(8) . ?
C10 C11 1.367(8) . ?
C4 C5 1.434(7) . ?
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
N1 O1 C15 109.3(3) . . ?
C17 N2 O3 118.7(3) . . ?
O2 C17 N2 121.9(4) . . ?
O2 C17 C15 120.3(3) . . ?
N2 C17 C15 117.7(3) . . ?
N2 O3 C18 108.6(4) . . ?
C1 N1 O1 109.9(4) . . ?
N1 C1 C13 118.1(5) . . ?
N1 C1 C2 132.7(5) . . ?
C13 C1 C2 109.2(4) . . ?
O1 C15 C17 110.8(3) . . ?
O1 C15 C14 113.5(3) . . ?
O1 C15 C16 101.6(3) . . ?
C14 C15 C17 110.7(4) . . ?
C16 C15 C17 108.3(4) . . ?
C16 C15 C14 111.5(4) . . ?
C13 C8 C7 109.8(4) . . ?
C9 C8 C7 131.9(5) . . ?
C9 C8 C13 118.3(6) . . ?
C6 C7 C8 131.0(4) . . ?
C6 C7 C2 121.9(5) . . ?
C2 C7 C8 107.1(4) . . ?
C8 C13 C1 106.1(5) . . ?
C12 C13 C1 133.7(5) . . ?
C12 C13 C8 120.2(5) . . ?
C11 C12 C13 120.0(6) . . ?
C7 C6 C5 119.1(5) . . ?
C7 C2 C1 107.8(5) . . ?
C3 C2 C1 134.8(5) . . ?
C3 C2 C7 117.4(5) . . ?
C2 C3 C4 123.6(5) . . ?
C11 C10 C9 121.1(6) . . ?
C8 C9 C10 120.1(5) . . ?
C3 C4 C5 117.7(6) . . ?
C6 C5 C4 120.4(6) . . ?
C12 C11 C10 120.3(7) . . ?
_shelx_res_file
;
20181222_mdl_zhp_ch9_67.res created by SHELXL-2014/7
TITL 20181222_MDL_ZHP_CH9_67 in Pbca #61
REM reset to Pbca #61
CELL 0.71073 15.01423 10.02283 21.5734 90 90 90
ZERR 14 0.00235 0.00105 0.00481 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 154 140 14 14
L.S. 99
PLAN 5
BOND
fmap 2
ACTA
REM
REM
REM
WGHT 0.120600
FVAR 3.48809
O2 4 0.243119 0.471517 0.076387 11.00000 0.07733 0.03709 =
0.15294 0.00184 -0.01665 0.00730
O1 4 0.407312 0.225382 0.120609 11.00000 0.08996 0.06456 =
0.08945 0.01604 -0.01168 -0.00518
N2 3 0.241824 0.248987 0.076435 11.00000 0.06452 0.03969 =
0.10737 -0.00077 -0.01750 0.00345
AFIX 43
H2 2 0.270127 0.175559 0.082550 11.00000 -1.20000
AFIX 0
C17 1 0.280048 0.365147 0.088159 11.00000 0.06537 0.04113 =
0.07977 -0.00140 0.00578 -0.00049
O3 4 0.155435 0.247860 0.054148 11.00000 0.06344 0.05766 =
0.12947 -0.00306 -0.00775 -0.00248
N1 3 0.370771 0.166467 0.171448 11.00000 0.07544 0.07786 =
0.07630 -0.00385 -0.00237 -0.00224
C1 1 0.403768 0.042585 0.178318 11.00000 0.07647 0.05649 =
0.09734 -0.01277 -0.02728 0.00348
C15 1 0.373529 0.363624 0.115291 11.00000 0.07616 0.03508 =
0.08155 0.00020 -0.00601 0.00485
C8 1 0.421438 -0.158728 0.227338 11.00000 0.07964 0.06101 =
0.07758 0.00084 -0.02903 -0.00666
C7 1 0.480557 -0.158194 0.174445 11.00000 0.08361 0.04515 =
0.09412 0.00417 -0.04074 0.00006
C13 1 0.374237 -0.034813 0.230552 11.00000 0.08577 0.06269 =
0.08544 0.00914 -0.02929 -0.01012
C12 1 0.315277 -0.012035 0.277487 11.00000 0.08182 0.09236 =
0.10108 -0.02073 -0.01615 0.00136
AFIX 43
H12 2 0.284885 0.068692 0.279570 11.00000 -1.20000
AFIX 0
C6 1 0.539002 -0.252966 0.152935 11.00000 0.10289 0.06561 =
0.09395 0.00654 -0.03010 0.00556
AFIX 43
H6 2 0.546385 -0.333049 0.174093 11.00000 -1.20000
AFIX 0
C14 1 0.376531 0.439917 0.175464 11.00000 0.11050 0.05950 =
0.08021 -0.01336 -0.01286 0.00292
AFIX 137
H14A 2 0.336913 0.399134 0.204806 11.00000 -1.50000
H14B 2 0.358468 0.530505 0.168332 11.00000 -1.50000
H14C 2 0.436125 0.438703 0.191579 11.00000 -1.50000
AFIX 0
C2 1 0.468600 -0.033601 0.143638 11.00000 0.07917 0.08086 =
0.07187 0.00800 -0.01705 -0.01864
C16 1 0.436116 0.421640 0.068368 11.00000 0.07647 0.06380 =
0.11328 0.00692 0.00182 0.00261
AFIX 137
H16A 2 0.494776 0.427484 0.085865 11.00000 -1.50000
H16B 2 0.416102 0.509155 0.056834 11.00000 -1.50000
H16C 2 0.437563 0.365445 0.032346 11.00000 -1.50000
AFIX 0
C3 1 0.516785 -0.011907 0.091811 11.00000 0.09305 0.07528 =
0.10653 -0.00831 -0.01326 0.01067
AFIX 43
H3 2 0.510057 0.069341 0.071523 11.00000 -1.20000
AFIX 0
C10 1 0.345930 -0.225599 0.318623 11.00000 0.12709 0.09918 =
0.09505 0.01410 -0.02103 -0.02388
AFIX 43
H10 2 0.335747 -0.289744 0.348954 11.00000 -1.20000
AFIX 0
C18 1 0.158271 0.243773 -0.010738 11.00000 0.11814 0.11638 =
0.13309 0.02790 -0.04902 -0.02382
AFIX 137
H18A 2 0.098691 0.240054 -0.026796 11.00000 -1.50000
H18B 2 0.190597 0.166098 -0.023844 11.00000 -1.50000
H18C 2 0.187469 0.322367 -0.026035 11.00000 -1.50000
AFIX 0
C9 1 0.405934 -0.251536 0.272039 11.00000 0.10765 0.07245 =
0.08539 0.01084 -0.02653 -0.01332
AFIX 43
H9 2 0.435970 -0.332658 0.271087 11.00000 -1.20000
AFIX 0
C4 1 0.575502 -0.103725 0.067276 11.00000 0.09640 0.10943 =
0.09451 0.00244 -0.00366 -0.01524
AFIX 43
H4 2 0.606858 -0.085845 0.031039 11.00000 -1.20000
AFIX 0
C5 1 0.586499 -0.227696 0.099598 11.00000 0.10997 0.09159 =
0.11514 -0.02135 -0.02364 0.01130
AFIX 43
H5 2 0.625935 -0.291386 0.084448 11.00000 -1.20000
AFIX 0
C11 1 0.300965 -0.107122 0.321130 11.00000 0.12439 0.13197 =
0.09318 0.01852 -0.00928 -0.03350
AFIX 43
H11 2 0.260384 -0.091628 0.352892 11.00000 -1.20000
AFIX 0
HKLF 4
REM 20181222_MDL_ZHP_CH9_67 in Pbca #61
REM R1 = 0.0871 for 1287 Fo > 4sig(Fo) and 0.2084 for all 3794 data
REM 211 parameters refined using 0 restraints
END
WGHT 0.1207 0.0000
REM Highest difference peak 0.384, deepest hole -0.239, 1-sigma level 0.048
Q1 1 0.4373 0.1330 0.1212 11.00000 0.05 0.38
Q2 1 0.6301 -0.1618 0.0466 11.00000 0.05 0.21
Q3 1 0.3411 0.0638 0.2369 11.00000 0.05 0.18
Q4 1 0.4457 0.0427 0.1377 11.00000 0.05 0.17
Q5 1 0.6102 -0.3171 0.0916 11.00000 0.05 0.16
;
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9 -11 0-17.1518 119.327 2
9 -11 -1 470.559 160.888 1
9 -11 1 113.270 314.621 1
9 -11 -1 22.9147 99.2935 2
9 -11 1-102.600 209.579 2
9 -11 -2-892.429 735.414 1
9 -11 -2 579.802 714.741 2
9 -11 2 282.808 347.306 2
9 -11 2-163.689 320.426 1
9 -11 -3-53.2743 152.216 2
9 -11 3-318.587 365.701 2
9 -11 3 119.525 519.921 1
9 -11 4-1.68381 32.6298 1
9 -11 4 55.8970 186.374 2
9 -11 5 339.539 242.183 2
9 -11 6 158.520 252.507 2
9 -11 7-521.057 457.553 2
9 -11 8-31.9938 113.195 2
9 -11 9 225.706 301.825 2
9 -11 10-56.5325 151.921 2
10 -11 0 175.655 363.680 2
10 -11 -1-244.589 334.319 2
10 -11 1-286.400 361.275 2
10 -11 -2 314.787 382.709 2
10 -11 2 136.530 376.080 2
10 -11 -3 551.040 498.754 2
10 -11 3-107.725 220.048 2
10 -11 -4-359.850 410.198 2
10 -11 4 381.518 513.802 2
10 -11 5-291.298 355.597 2
10 -11 6-6.85865 54.2605 2
10 -11 7 125.068 332.787 2
10 -11 8-327.956 375.797 2
11 -11 0-181.591 296.351 2
11 -11 -1-345.074 409.239 2
11 -11 1 298.009 364.140 2
11 -11 -2 265.254 360.774 2
11 -11 2-1.28085 108.192 2
11 -11 -3 90.4685 212.600 2
11 -11 3 45.9670 104.979 2
11 -11 -4 196.698 313.321 2
11 -11 4 626.423 664.884 2
11 -11 -5 207.746 499.600 2
11 -11 5-446.930 455.203 2
12 -11 -1 426.783 520.436 2
12 -11 -2 211.630 332.641 2
0 -12 0 1518.66 1090.38 1
0 -12 1 150.102 341.785 1
0 -12 -1-951.579 803.268 1
0 -12 -2 131.113 377.239 1
0 -12 2 1.94648 490.360 1
0 -12 -3 1.69471 295.569 1
0 -12 3-410.861 548.118 1
0 -12 4 222.743 399.040 1
0 -12 -4 1030.09 820.943 1
0 -12 -5 465.989 580.084 1
0 -12 -6 276.389 525.613 1
0 -12 -7-2322.06 1139.28 1
0 -12 -8-530.541 533.768 1
0 -12 -9 34.6354 396.396 1
0 -12 -10-156.074 280.817 1
0 -12 -11 450.517 465.330 1
0 -12 -12 40.2324 282.521 1
0 -12 -13 102.001 429.882 1
-1 -12 0-387.098 513.986 1
1 -12 0-214.291 394.151 1
1 -12 1 347.936 349.130 1
1 -12 -1-1.85797 267.019 1
-1 -12 1-57.8636 201.394 1
-1 -12 -1-1.74006 353.657 1
-1 -12 2 20.9238 122.254 1
1 -12 -2-151.946 321.270 1
-1 -12 -2-581.942 605.391 1
1 -12 2 294.594 375.399 1
-1 -12 -3 219.072 358.637 1
-1 -12 3-128.620 362.589 1
1 -12 -3-513.872 581.758 1
1 -12 3-509.992 612.911 1
1 -12 4-469.985 581.864 1
1 -12 -4 449.473 703.093 1
-1 -12 -4 179.371 324.134 1
1 -12 5-878.238 780.063 1
1 -12 -5 470.532 536.365 1
-1 -12 -5 481.521 668.830 1
1 -12 -6-44.2098 161.905 1
-1 -12 -6 433.091 596.770 1
1 -12 -7-1240.72 847.946 1
-1 -12 -7-1193.76 796.278 1
1 -12 -8-782.846 660.833 1
-1 -12 -8-494.565 502.335 1
1 -12 -9-1390.41 870.527 1
-1 -12 -9-954.902 690.586 1
1 -12 -10 40.3363 390.597 1
-1 -12 -10 123.937 283.390 1
1 -12 -11 241.556 502.924 1
-1 -12 -11-250.295 337.940 1
1 -12 -12 31.9727 290.082 1
-1 -12 -12 25.4542 44.8423 1
-2 -12 0 141.026 303.652 1
2 -12 0 267.910 528.036 1
2 -12 -1-362.968 508.947 1
-2 -12 1-206.366 372.915 1
-2 -12 -1 29.9691 136.886 1
2 -12 1 271.983 448.666 1
2 -12 -2 105.702 628.621 1
2 -12 2-120.470 298.906 1
-2 -12 -2 488.960 451.269 1
-2 -12 2-246.809 413.171 1
-2 -12 -3-273.418 397.134 1
-2 -12 3 150.004 580.234 1
2 -12 3-937.427 828.297 1
2 -12 -3-1.80198 115.816 1
2 -12 4 113.641 51.9064 1
2 -12 -4 172.383 348.762 1
-2 -12 -4-107.097 244.587 1
2 -12 5-709.624 695.442 1
2 -12 -5 1.67957 582.230 1
-2 -12 -5 290.456 383.310 1
2 -12 -6-1532.09 971.998 1
-2 -12 -6 450.933 584.294 1
2 -12 6-963.170 787.328 1
2 -12 -7 151.769 300.171 1
-2 -12 -7-1391.71 836.281 1
2 -12 -8-968.359 750.015 1
-2 -12 -8-1089.52 728.479 1
2 -12 -9 34.3010 236.558 1
-2 -12 -9-1058.05 707.013 1
2 -12 -10-854.115 681.992 1
-2 -12 -10 206.642 475.325 1
2 -12 -11 1.37622 391.047 1
-2 -12 -11-228.641 314.086 1
-3 -12 0 42.7075 379.311 1
3 -12 0 168.271 286.265 1
3 -12 -1-422.176 552.830 1
3 -12 1-403.778 547.834 1
-3 -12 -1 17.4237 430.825 1
-3 -12 1 258.793 656.727 1
-3 -12 2 214.022 108.391 1
-3 -12 -2 205.228 317.657 1
3 -12 2 53.3940 365.570 1
3 -12 -2 380.572 518.898 1
-3 -12 -3 198.263 388.377 1
3 -12 3-95.3145 263.865 1
3 -12 -3 541.239 582.764 1
3 -12 -4 826.082 854.001 1
3 -12 4-468.793 575.708 1
-3 -12 -4 98.0849 321.284 1
3 -12 5 12.4898 91.4805 1
3 -12 -5 91.1989 191.554 1
-3 -12 -5 287.179 381.310 1
3 -12 6-463.303 541.401 1
-3 -12 -6 195.729 308.665 1
3 -12 -7-1314.22 894.291 1
-3 -12 -7-540.074 505.886 1
3 -12 7-585.267 588.036 1
3 -12 -8-655.298 624.863 1
-3 -12 -8-978.413 670.344 1
-3 -12 -9 14.2336 139.816 1
3 -12 -9-557.804 568.917 1
4 -12 0 350.635 483.421 1
-4 -12 0-319.032 431.796 1
4 -12 -1 539.751 846.357 1
-4 -12 1-1169.93 841.996 1
4 -12 1 140.710 380.605 1
-4 -12 -1 74.3502 395.104 1
-4 -12 -2 336.580 314.012 1
4 -12 2 951.425 1051.11 1
-4 -12 2-663.797 648.049 1
4 -12 -2 135.232 402.021 1
-4 -12 -3 56.1587 215.638 1
4 -12 -3 1082.66 994.212 1
4 -12 3 575.527 1001.69 1
4 -12 4-256.461 423.061 1
4 -12 -4 652.699 864.244 1
-4 -12 -4 354.385 418.716 1
4 -12 5-232.388 393.458 1
-4 -12 -5 258.767 350.230 1
4 -12 -6-1562.22 1003.01 1
-4 -12 -6 224.382 418.083 1
4 -12 -7-1247.58 879.864 1
5 -12 0-357.543 510.787 1
-5 -12 0-484.433 515.211 1
-5 -12 -1 439.210 481.854 1
5 -12 1 592.037 776.187 1
-5 -12 1-699.069 633.006 1
5 -12 -1 36.4893 435.606 1
-5 -12 2-1020.46 779.243 1
5 -12 2 542.192 627.906 1
-5 -12 -2-137.109 263.079 1
5 -12 -2 353.008 852.577 1
-5 -12 -3 74.6162 328.852 1
5 -12 -3 270.305 657.048 1
5 -12 3-53.3914 195.530 1
5 -12 -4 166.001 92.5107 1
-5 -12 -4-175.791 285.872 1
5 -12 -5-665.259 665.727 1
-6 -12 0-113.110 242.055 1
-6 -12 -1-126.872 250.930 1
-6 -12 1-1216.15 808.349 1
-6 -12 2-943.365 727.757 1
0 -13 0 412.844 570.777 1
0 -13 -1-393.570 536.620 1
0 -13 -2 22.7081 465.300 1
0 -13 -3 14.6624 311.660 1
0 -13 -4-269.326 420.571 1
0 -13 -5-176.805 335.969 1
-1 -13 0 341.911 498.020 1
-1 -13 -1-294.741 454.395 1
-1 -13 1 111.502 1203.76 1
-1 -13 -2 1452.02 1044.79 1
-1 -13 2 2.03579 147.611 1
-1 -13 -3 13.8683 561.120 1
-1 -13 -4-53.4313 183.038 1
-1 -13 -5 145.702 466.381 1
-1 -13 -6-987.667 762.537 1
-1 -13 -7-807.484 680.985 1
-1 -13 -8-765.042 649.512 1
-2 -13 0 872.046 777.838 1
-2 -13 1-1.91170 1105.90 1
-2 -13 -1 40.9230 165.358 1
-2 -13 -2-466.665 546.325 1
-2 -13 2-17.7050 114.366 1
-2 -13 -3 49.3884 174.737 1
-2 -13 -4 101.759 246.492 1
-2 -13 -5 30.4960 191.495 1
-2 -13 -6-419.344 483.912 1
-2 -13 -7-494.462 517.377 1
-3 -13 0 186.127 447.556 1
-3 -13 1 1.82146 780.540 1
-3 -13 -1-53.4696 183.170 1
-3 -13 -2 153.081 601.458 1
-3 -13 2 37.6587 379.200 1
-3 -13 3-883.210 802.378 1
-3 -13 -3 411.099 488.457 1
-3 -13 -4 150.842 290.859 1
-3 -13 -5 348.260 432.934 1
-3 -13 -6-938.314 701.952 1
-4 -13 0-87.2385 232.215 1
-4 -13 1-453.304 539.620 1
-4 -13 -1-280.100 407.988 1
-4 -13 -2 132.907 476.442 1
-4 -13 2 259.581 417.743 1
-4 -13 -3 106.827 273.478 1
-4 -13 3-705.168 701.005 1
-4 -13 -4 161.225 485.994 1
-5 -13 0 365.254 459.771 1
-5 -13 1 342.481 455.816 1
-5 -13 2 23.5049 121.735 1
-5 -13 3-522.089 585.099 1
0 0 0 0.00 0.00 0
TITL 20181222_MDL_ZHP_CH9_67 in Pbca
REM Pbca (#61, found as Pcab in ba-c setting)
CELL 0.71073 15.014229 10.022830 21.573401 90.0000 90.0000 90.0000
ZERR 14.00 0.002353 0.001054 0.004807 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 N O
UNIT 154.00 140.00 14.00 14.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 81739
_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 1.808
_oxdiff_exptl_absorpt_empirical_full_min 0.408
#######################################################################
#
# 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_20180718_MDL_ZHP_CCH_8_53
_database_code_depnum_ccdc_archive 'CCDC 1938293'
loop_
_audit_author_name
_audit_author_address
'Dong-Liang Mo'
;Guangxi Normal University
China
;
_audit_update_record
;
2019-07-04 deposited with the CCDC. 2020-09-25 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C17 H16 N2 O2'
_chemical_formula_weight 280.32
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 11.2384(6)
_cell_length_b 10.3430(5)
_cell_length_c 13.5036(8)
_cell_angle_alpha 90
_cell_angle_beta 107.740(6)
_cell_angle_gamma 90
_cell_volume 1494.99(15)
_cell_formula_units_Z 4
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used 3082
_cell_measurement_theta_min 3.633
_cell_measurement_theta_max 28.339
_exptl_crystal_description block
_exptl_crystal_colour ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.245
_exptl_crystal_F_000 592
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.280
_exptl_crystal_size_mid 0.250
_exptl_crystal_size_min 0.230
_exptl_absorpt_coefficient_mu 0.083
_shelx_estimated_absorpt_T_min 0.977
_shelx_estimated_absorpt_T_max 0.981
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_process_details ?
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 296(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 11821
_diffrn_reflns_av_unetI/netI 0.0278
_diffrn_reflns_av_R_equivalents 0.0250
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 3.442
_diffrn_reflns_theta_max 29.059
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total 3611
_reflns_number_gt 2519
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_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.
;
_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.6626P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 3611
_refine_ls_number_parameters 192
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0851
_refine_ls_R_factor_gt 0.0593
_refine_ls_wR_factor_ref 0.1658
_refine_ls_wR_factor_gt 0.1497
_refine_ls_goodness_of_fit_ref 1.055
_refine_ls_restrained_S_all 1.055
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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 0.30436(12) 0.83661(14) 0.04972(11) 0.0530(4) Uani 1 1 d . . . . .
N2 N 0.19816(15) 0.76628(17) 0.05126(13) 0.0500(4) Uani 1 1 d . . . . .
C3 C 0.09842(16) 0.81417(19) -0.01505(14) 0.0429(4) Uani 1 1 d . . . . .
C4 C -0.11604(17) 0.8251(2) -0.09708(15) 0.0459(5) Uani 1 1 d . . . . .
O5 O 0.52457(16) 0.57843(16) 0.12793(12) 0.0692(5) Uani 1 1 d . . . . .
N6 N 0.39638(16) 0.63770(19) -0.02764(13) 0.0567(5) Uani 1 1 d . . . . .
H6A H 0.4166 0.5721 -0.0582 0.068 Uiso 1 1 calc R U . . .
H6B H 0.3428 0.6928 -0.0629 0.068 Uiso 1 1 calc R U . . .
C7 C 0.07459(17) 0.91921(19) -0.09190(14) 0.0433(4) Uani 1 1 d . . . . .
C8 C -0.02428(18) 0.7573(2) -0.02165(15) 0.0473(5) Uani 1 1 d . . . . .
C9 C -0.05512(17) 0.92445(19) -0.14147(14) 0.0447(4) Uani 1 1 d . . . . .
C10 C 0.41478(18) 0.7773(2) 0.12105(16) 0.0522(5) Uani 1 1 d . . . . .
C11 C 0.44773(17) 0.6538(2) 0.07374(15) 0.0464(5) Uani 1 1 d . . . . .
C12 C 0.1539(2) 1.0028(2) -0.12066(19) 0.0614(6) Uani 1 1 d . . . . .
H12 H 0.2397 0.9999 -0.0882 0.074 Uiso 1 1 calc R U . . .
C13 C -0.2400(2) 0.7917(3) -0.11813(19) 0.0641(6) Uani 1 1 d . . . . .
H13 H -0.3019 0.8367 -0.1677 0.077 Uiso 1 1 calc R U . . .
C14 C -0.1045(2) 1.0132(2) -0.21882(18) 0.0630(6) Uani 1 1 d . . . . .
H14 H -0.1902 1.0172 -0.2515 0.076 Uiso 1 1 calc R U . . .
C15 C 0.3984(2) 0.7506(3) 0.22576(17) 0.0791(9) Uani 1 1 d . . . . .
H15A H 0.3768 0.8293 0.2539 0.119 Uiso 1 1 calc R U . . .
H15B H 0.4750 0.7172 0.2719 0.119 Uiso 1 1 calc R U . . .
H15C H 0.3330 0.6882 0.2183 0.119 Uiso 1 1 calc R U . . .
C16 C -0.0550(2) 0.6565(3) 0.0320(2) 0.0705(7) Uani 1 1 d . . . . .
H16 H 0.0062 0.6116 0.0823 0.085 Uiso 1 1 calc R U . . .
C17 C -0.0245(3) 1.0961(3) -0.2469(2) 0.0836(8) Uani 1 1 d . . . . .
H17 H -0.0567 1.1567 -0.2991 0.100 Uiso 1 1 calc R U . . .
C18 C 0.1028(3) 1.0906(3) -0.1988(2) 0.0824(8) Uani 1 1 d . . . . .
H18 H 0.1550 1.1472 -0.2194 0.099 Uiso 1 1 calc R U . . .
C19 C 0.5170(2) 0.8761(3) 0.1267(3) 0.0877(9) Uani 1 1 d . . . . .
H19A H 0.5219 0.8923 0.0580 0.132 Uiso 1 1 calc R U . . .
H19B H 0.5957 0.8432 0.1697 0.132 Uiso 1 1 calc R U . . .
H19C H 0.4980 0.9552 0.1558 0.132 Uiso 1 1 calc R U . . .
C20 C -0.2703(2) 0.6903(3) -0.0642(2) 0.0861(9) Uani 1 1 d . . . . .
H20 H -0.3536 0.6666 -0.0778 0.103 Uiso 1 1 calc R U . . .
C21 C -0.1794(3) 0.6236(3) 0.0094(2) 0.0897(9) Uani 1 1 d . . . . .
H21 H -0.2021 0.5552 0.0445 0.108 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 0.0377(7) 0.0554(8) 0.0602(9) 0.0037(7) 0.0065(6) 0.0006(6)
N2 0.0391(9) 0.0551(10) 0.0537(10) -0.0053(8) 0.0112(7) -0.0026(7)
C3 0.0355(10) 0.0493(10) 0.0410(10) -0.0071(8) 0.0073(8) 0.0035(8)
C4 0.0366(9) 0.0553(11) 0.0422(10) -0.0066(9) 0.0067(8) 0.0011(8)
O5 0.0728(10) 0.0757(11) 0.0499(9) 0.0002(8) 0.0052(8) 0.0310(9)
N6 0.0561(11) 0.0686(12) 0.0426(9) -0.0016(8) 0.0110(8) 0.0150(9)
C7 0.0393(10) 0.0486(10) 0.0418(10) -0.0067(8) 0.0124(8) 0.0009(8)
C8 0.0389(10) 0.0533(11) 0.0465(11) -0.0013(9) 0.0083(8) -0.0017(8)
C9 0.0423(10) 0.0529(11) 0.0377(9) -0.0050(8) 0.0104(8) 0.0049(8)
C10 0.0353(10) 0.0606(12) 0.0519(12) -0.0054(10) 0.0002(8) 0.0071(9)
C11 0.0373(10) 0.0576(12) 0.0428(10) -0.0005(9) 0.0097(8) 0.0024(9)
C12 0.0520(12) 0.0671(14) 0.0665(14) 0.0068(11) 0.0201(11) -0.0025(11)
C13 0.0364(11) 0.0854(17) 0.0626(14) 0.0007(12) 0.0031(10) -0.0035(11)
C14 0.0569(13) 0.0745(15) 0.0530(12) 0.0109(11) 0.0099(10) 0.0139(12)
C15 0.0626(15) 0.120(2) 0.0452(13) -0.0110(14) 0.0026(11) 0.0327(15)
C16 0.0541(14) 0.0760(16) 0.0728(16) 0.0189(13) 0.0066(11) -0.0066(12)
C17 0.088(2) 0.0878(19) 0.0739(17) 0.0380(15) 0.0227(15) 0.0124(16)
C18 0.0752(18) 0.091(2) 0.0839(19) 0.0259(16) 0.0292(15) -0.0066(15)
C19 0.0501(14) 0.0721(17) 0.120(2) -0.0041(16) -0.0045(15) -0.0090(12)
C20 0.0465(14) 0.110(2) 0.094(2) 0.0113(18) 0.0099(13) -0.0239(14)
C21 0.0671(17) 0.098(2) 0.097(2) 0.0281(17) 0.0149(15) -0.0268(15)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 N2 1.403(2) . ?
O1 C10 1.454(2) . ?
N2 C3 1.301(2) . ?
C3 C7 1.470(3) . ?
C3 C8 1.477(3) . ?
C4 C13 1.378(3) . ?
C4 C8 1.397(3) . ?
C4 C9 1.461(3) . ?
O5 C11 1.226(2) . ?
N6 C11 1.324(2) . ?
C7 C12 1.379(3) . ?
C7 C9 1.408(3) . ?
C8 C16 1.373(3) . ?
C9 C14 1.374(3) . ?
C10 C15 1.506(3) . ?
C10 C19 1.523(3) . ?
C10 C11 1.524(3) . ?
C12 C18 1.378(3) . ?
C13 C20 1.377(4) . ?
C14 C17 1.377(4) . ?
C16 C21 1.379(3) . ?
C17 C18 1.380(4) . ?
C20 C21 1.374(4) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 O1 C10 109.23(15) . . ?
C3 N2 O1 110.54(16) . . ?
N2 C3 C7 134.51(18) . . ?
N2 C3 C8 118.87(18) . . ?
C7 C3 C8 106.62(15) . . ?
C13 C4 C8 120.0(2) . . ?
C13 C4 C9 131.47(19) . . ?
C8 C4 C9 108.54(17) . . ?
C12 C7 C9 120.42(19) . . ?
C12 C7 C3 131.88(18) . . ?
C9 C7 C3 107.68(16) . . ?
C16 C8 C4 121.15(19) . . ?
C16 C8 C3 130.65(19) . . ?
C4 C8 C3 108.20(17) . . ?
C14 C9 C7 120.5(2) . . ?
C14 C9 C4 130.59(19) . . ?
C7 C9 C4 108.95(17) . . ?
O1 C10 C15 112.06(17) . . ?
O1 C10 C19 103.21(18) . . ?
C15 C10 C19 112.5(2) . . ?
O1 C10 C11 110.08(16) . . ?
C15 C10 C11 110.8(2) . . ?
C19 C10 C11 107.91(19) . . ?
O5 C11 N6 122.88(19) . . ?
O5 C11 C10 119.98(17) . . ?
N6 C11 C10 116.99(18) . . ?
C18 C12 C7 118.3(2) . . ?
C20 C13 C4 118.6(2) . . ?
C9 C14 C17 118.6(2) . . ?
C8 C16 C21 118.1(2) . . ?
C14 C17 C18 121.0(2) . . ?
C12 C18 C17 121.2(2) . . ?
C21 C20 C13 121.0(2) . . ?
C20 C21 C16 121.1(3) . . ?
_refine_diff_density_max 0.278
_refine_diff_density_min -0.192
_refine_diff_density_rms 0.038
_shelx_res_file
;
20180718_MDL_ZHP_CCH_8_53.res created by SHELXL-2014/7
TITL 20180718_MDL_ZHP_CCH_8_53 in P21/c #14
REM reset to P21/c #14
CELL 0.71073 11.238378 10.342987 13.50356 90 107.7403 90
ZERR 4 0.000585 0.000538 0.000762 0 0.0057 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 68 64 8 8
L.S. 4
PLAN 20
acta
temp 23
size 0.28 0.25 0.23
BOND
fmap 2
REM
REM
REM
WGHT 0.057600 0.662600
FVAR 7.00877
O1 4 0.304361 0.836608 0.049722 11.00000 0.03774 0.05535 =
0.06023 0.00374 0.00651 0.00064
N2 3 0.198160 0.766277 0.051261 11.00000 0.03911 0.05512 =
0.05371 -0.00526 0.01123 -0.00264
C3 1 0.098422 0.814167 -0.015046 11.00000 0.03548 0.04929 =
0.04095 -0.00709 0.00734 0.00347
C4 1 -0.116045 0.825090 -0.097085 11.00000 0.03661 0.05529 =
0.04218 -0.00659 0.00673 0.00105
O5 4 0.524573 0.578427 0.127932 11.00000 0.07279 0.07574 =
0.04993 0.00022 0.00522 0.03101
N6 3 0.396376 0.637696 -0.027641 11.00000 0.05614 0.06860 =
0.04262 -0.00163 0.01098 0.01503
AFIX 93
H6A 2 0.416596 0.572113 -0.058232 11.00000 -1.20000
H6B 2 0.342800 0.692826 -0.062893 11.00000 -1.20000
AFIX 0
C7 1 0.074592 0.919212 -0.091904 11.00000 0.03933 0.04863 =
0.04184 -0.00669 0.01238 0.00087
C8 1 -0.024275 0.757303 -0.021648 11.00000 0.03887 0.05326 =
0.04645 -0.00133 0.00827 -0.00173
C9 1 -0.055117 0.924450 -0.141466 11.00000 0.04234 0.05289 =
0.03768 -0.00502 0.01037 0.00493
C10 1 0.414779 0.777296 0.121045 11.00000 0.03526 0.06056 =
0.05187 -0.00539 0.00020 0.00707
C11 1 0.447734 0.653790 0.073741 11.00000 0.03726 0.05755 =
0.04284 -0.00053 0.00970 0.00243
C12 1 0.153879 1.002761 -0.120657 11.00000 0.05198 0.06705 =
0.06650 0.00681 0.02010 -0.00248
AFIX 43
H12 2 0.239652 0.999890 -0.088152 11.00000 -1.20000
AFIX 0
C13 1 -0.239962 0.791731 -0.118129 11.00000 0.03637 0.08535 =
0.06256 0.00073 0.00311 -0.00346
AFIX 43
H13 2 -0.301854 0.836744 -0.167701 11.00000 -1.20000
AFIX 0
C14 1 -0.104472 1.013211 -0.218816 11.00000 0.05686 0.07450 =
0.05299 0.01095 0.00994 0.01393
AFIX 43
H14 2 -0.190163 1.017209 -0.251501 11.00000 -1.20000
AFIX 0
C15 1 0.398412 0.750561 0.225756 11.00000 0.06256 0.12029 =
0.04515 -0.01101 0.00258 0.03269
AFIX 137
H15A 2 0.376821 0.829262 0.253858 11.00000 -1.50000
H15B 2 0.475011 0.717161 0.271882 11.00000 -1.50000
H15C 2 0.332971 0.688217 0.218274 11.00000 -1.50000
AFIX 0
C16 1 -0.055044 0.656478 0.032036 11.00000 0.05410 0.07596 =
0.07278 0.01893 0.00657 -0.00659
AFIX 43
H16 2 0.006235 0.611623 0.082265 11.00000 -1.20000
AFIX 0
C17 1 -0.024483 1.096090 -0.246935 11.00000 0.08774 0.08775 =
0.07394 0.03803 0.02272 0.01244
AFIX 43
H17 2 -0.056668 1.156659 -0.299143 11.00000 -1.20000
AFIX 0
C18 1 0.102752 1.090605 -0.198786 11.00000 0.07523 0.09146 =
0.08395 0.02589 0.02925 -0.00662
AFIX 43
H18 2 0.154968 1.147232 -0.219439 11.00000 -1.20000
AFIX 0
C19 1 0.517041 0.876121 0.126664 11.00000 0.05011 0.07205 =
0.12048 -0.00414 -0.00446 -0.00902
AFIX 137
H19A 2 0.521926 0.892303 0.058006 11.00000 -1.50000
H19B 2 0.595663 0.843159 0.169680 11.00000 -1.50000
H19C 2 0.498011 0.955213 0.155848 11.00000 -1.50000
AFIX 0
C20 1 -0.270277 0.690326 -0.064223 11.00000 0.04648 0.11010 =
0.09415 0.01128 0.00994 -0.02388
AFIX 43
H20 2 -0.353552 0.666627 -0.077832 11.00000 -1.20000
AFIX 0
C21 1 -0.179366 0.623639 0.009355 11.00000 0.06706 0.09794 =
0.09735 0.02805 0.01486 -0.02681
AFIX 43
H21 2 -0.202092 0.555184 0.044451 11.00000 -1.20000
AFIX 0
HKLF 4
REM 20180718_MDL_ZHP_CCH_8_53 in P21/c #14
REM R1 = 0.0593 for 2519 Fo > 4sig(Fo) and 0.0851 for all 3611 data
REM 192 parameters refined using 0 restraints
END
WGHT 0.0576 0.6632
REM Highest difference peak 0.278, deepest hole -0.192, 1-sigma level 0.038
Q1 1 0.2481 0.7188 0.1062 11.00000 0.05 0.28
Q2 1 0.2145 0.8437 0.0082 11.00000 0.05 0.26
Q3 1 0.4457 0.8613 0.1653 11.00000 0.05 0.25
Q4 1 0.3576 0.6455 0.2424 11.00000 0.05 0.22
Q5 1 0.3641 0.7254 0.1482 11.00000 0.05 0.20
Q6 1 0.0979 0.8595 -0.0603 11.00000 0.05 0.16
Q7 1 -0.0957 0.8853 -0.1107 11.00000 0.05 0.16
Q8 1 0.0071 0.9386 -0.1155 11.00000 0.05 0.14
Q9 1 0.0277 0.7886 -0.0209 11.00000 0.05 0.14
Q10 1 -0.0770 0.7942 -0.0541 11.00000 0.05 0.14
Q11 1 0.1381 1.2156 -0.1766 11.00000 0.05 0.13
Q12 1 0.5667 0.6199 0.0841 11.00000 0.05 0.13
Q13 1 0.4537 0.6769 0.2754 11.00000 0.05 0.13
Q14 1 0.2852 0.8549 -0.0953 11.00000 0.05 0.12
Q15 1 0.4566 0.5741 0.1087 11.00000 0.05 0.11
Q16 1 0.4025 0.8814 0.2464 11.00000 0.05 0.11
Q17 1 0.3179 0.7641 0.2485 11.00000 0.05 0.11
Q18 1 0.5749 0.8700 0.2248 11.00000 0.05 0.11
Q19 1 0.2074 1.1918 -0.1058 11.00000 0.05 0.11
Q20 1 0.3848 0.5162 0.1304 11.00000 0.05 0.11
;
_shelx_res_checksum 5658
_shelx_hkl_file
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0 0 0 0.00 0.00 0
TITL 20180718_MDL_ZHP_CCH_8_53 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 11.238378 10.342987 13.503560 90.0000 107.7403 90.0000
ZERR 6.00 0.000585 0.000538 0.000762 0.0000 0.0057 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O
UNIT 66.00 60.00 6.00 6.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 1924