# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024
#######################################################################
#
# 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_mo_cns_js_186_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2319368'
loop_
_audit_author_name
_audit_author_address
'Charlotte Stindt'
;University of Groningen
Netherlands
;
_audit_update_record
;
2023-12-18 deposited with the CCDC. 2024-03-27 downloaded from the CCDC.
;
_audit_creation_date 2023-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C24 H28 O2'
_chemical_formula_sum 'C24 H28 O2'
_chemical_formula_weight 348.46
_chemical_absolute_configuration ?
_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'
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 monoclinic
_space_group_IT_number 9
_space_group_name_H-M_alt 'C 1 c 1'
_space_group_name_Hall 'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
_cell_length_a 11.361(4)
_cell_length_b 20.063(7)
_cell_length_c 9.862(4)
_cell_angle_alpha 90
_cell_angle_beta 116.079(16)
_cell_angle_gamma 90
_cell_volume 2019.1(13)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 6872
_cell_measurement_temperature 293
_cell_measurement_theta_max 24.20
_cell_measurement_theta_min 2.50
_shelx_estimated_absorpt_T_max 0.990
_shelx_estimated_absorpt_T_min 0.975
_exptl_absorpt_coefficient_mu 0.071
_exptl_absorpt_correction_T_max 0.6699
_exptl_absorpt_correction_T_min 0.5708
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1248 before and 0.0973 after correction.
The Ratio of minimum to maximum transmission is 0.8521.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.146
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 752
_exptl_crystal_size_max 0.355
_exptl_crystal_size_mid 0.156
_exptl_crystal_size_min 0.139
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1198
_diffrn_reflns_av_unetI/netI 0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 55231
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.561
_diffrn_reflns_theta_min 3.643
_diffrn_ambient_temperature 293
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_source_current 30.0
_diffrn_source_power 1.5
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.995
_reflns_Friedel_fraction_full 0.992
_reflns_Friedel_fraction_max 0.995
_reflns_number_gt 4051
_reflns_number_total 5625
_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 'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max 0.155
_refine_diff_density_min -0.140
_refine_diff_density_rms 0.029
_refine_ls_abs_structure_details
;
Flack x determined using 1509 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack -0.1(9)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 241
_refine_ls_number_reflns 5625
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0843
_refine_ls_R_factor_gt 0.0547
_refine_ls_restrained_S_all 1.026
_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^)+(0.0371P)^2^+0.8110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1097
_refine_ls_wR_factor_ref 0.1258
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C00E(H00N,H00O), C00N(H00U,H00V)
2.b Aromatic/amide H refined with riding coordinates:
C006(H006), C00A(H00G), C00L(H00S), C00M(H00T), C00O(H00W), C00P(H00X)
2.c Idealised Me refined as rotating group:
C008(H00A,H00B,H00C), C009(H00D,H00E,H00F), C00B(H00H,H00I,H00J), C00D(H00K,
H00L,H00M), C00G(H00P,H00Q,H00R), C00Q(H00Y,H,HA)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary iterative
_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
C001 C 0.4474(2) 0.76003(13) 0.4468(3) 0.0389(6) Uani 1 1 d . . . . .
O002 O 0.5994(3) 0.52801(12) 0.4816(3) 0.0810(8) Uani 1 1 d . . . . .
C003 C 0.4645(3) 0.69431(14) 0.3894(3) 0.0416(6) Uani 1 1 d . . . . .
C004 C 0.4265(2) 0.77193(13) 0.5695(3) 0.0381(5) Uani 1 1 d . . . . .
O005 O 0.6111(3) 0.99441(13) 0.8003(4) 0.0937(10) Uani 1 1 d . . . . .
C006 C 0.5230(3) 0.63670(14) 0.4678(3) 0.0467(6) Uani 1 1 d . . . . .
H006 H 0.549870 0.634358 0.571403 0.056 Uiso 1 1 calc R U . . .
C007 C 0.4387(3) 0.83624(14) 0.6492(3) 0.0422(6) Uani 1 1 d . . . . .
C008 C 0.3601(3) 0.87235(16) 0.3062(4) 0.0599(8) Uani 1 1 d . . . . .
H00A H 0.277661 0.859584 0.303491 0.090 Uiso 1 1 calc R U . . .
H00B H 0.345055 0.894368 0.213534 0.090 Uiso 1 1 calc R U . . .
H00C H 0.404896 0.902081 0.389401 0.090 Uiso 1 1 calc R U . . .
C009 C 0.5835(4) 0.83037(19) 0.3522(5) 0.0710(10) Uani 1 1 d . . . . .
H00D H 0.624928 0.855011 0.444791 0.106 Uiso 1 1 calc R U . . .
H00E H 0.579131 0.857506 0.269951 0.106 Uiso 1 1 calc R U . . .
H00F H 0.633492 0.790904 0.358682 0.106 Uiso 1 1 calc R U . . .
C00A C 0.5247(3) 0.88905(14) 0.6713(3) 0.0493(7) Uani 1 1 d . . . . .
H00G H 0.578689 0.889847 0.622580 0.059 Uiso 1 1 calc R U . . .
C00B C 0.4870(4) 0.69501(18) 0.7951(4) 0.0644(9) Uani 1 1 d . . . . .
H00H H 0.547770 0.671374 0.769200 0.097 Uiso 1 1 calc R U . . .
H00I H 0.452654 0.665307 0.845245 0.097 Uiso 1 1 calc R U . . .
H00J H 0.531233 0.731410 0.861113 0.097 Uiso 1 1 calc R U . . .
C00C C 0.4435(3) 0.81056(15) 0.3252(4) 0.0481(7) Uani 1 1 d . . . . .
C00D C 0.2862(4) 0.66609(17) 0.5535(4) 0.0657(9) Uani 1 1 d . . . . .
H00K H 0.229597 0.683013 0.455145 0.099 Uiso 1 1 calc R U . . .
H00L H 0.234301 0.648846 0.600401 0.099 Uiso 1 1 calc R U . . .
H00M H 0.339862 0.631108 0.544155 0.099 Uiso 1 1 calc R U . . .
C00E C 0.2910(3) 0.76975(16) 0.6989(4) 0.0546(7) Uani 1 1 d . . . . .
H00N H 0.202339 0.773942 0.619528 0.066 Uiso 1 1 calc R U . . .
H00O H 0.287397 0.753652 0.789817 0.066 Uiso 1 1 calc R U . . .
C00F C 0.3614(3) 0.83439(15) 0.7269(3) 0.0486(7) Uani 1 1 d . . . . .
C00G C 0.7102(4) 0.9931(2) 0.7528(6) 0.0890(14) Uani 1 1 d . . . . .
H00P H 0.671921 0.995434 0.644607 0.134 Uiso 1 1 calc R U . . .
H00Q H 0.759295 0.952506 0.786159 0.134 Uiso 1 1 calc R U . . .
H00R H 0.767529 1.030497 0.794973 0.134 Uiso 1 1 calc R U . . .
C00H C 0.4297(3) 0.69801(16) 0.2352(3) 0.0548(7) Uani 1 1 d . . . . .
C00I C 0.5414(3) 0.58238(16) 0.3914(4) 0.0538(7) Uani 1 1 d . . . . .
C00J C 0.5285(3) 0.94060(16) 0.7674(4) 0.0616(9) Uani 1 1 d . . . . .
C00K C 0.3737(3) 0.72223(14) 0.6503(3) 0.0449(6) Uani 1 1 d . . . . .
C00L C 0.5022(4) 0.58557(18) 0.2378(4) 0.0638(9) Uani 1 1 d . . . . .
H00S H 0.512963 0.548962 0.186461 0.077 Uiso 1 1 calc R U . . .
C00M C 0.4464(4) 0.64403(19) 0.1603(4) 0.0681(10) Uani 1 1 d . . . . .
H00T H 0.420138 0.646493 0.056864 0.082 Uiso 1 1 calc R U . . .
C00N C 0.3806(4) 0.76705(18) 0.1811(4) 0.0682(10) Uani 1 1 d . . . . .
H00U H 0.285770 0.768824 0.137930 0.082 Uiso 1 1 calc R U . . .
H00V H 0.408340 0.781705 0.105881 0.082 Uiso 1 1 calc R U . . .
C00O C 0.3655(3) 0.88632(17) 0.8215(4) 0.0607(8) Uani 1 1 d . . . . .
H00W H 0.312929 0.885227 0.871921 0.073 Uiso 1 1 calc R U . . .
C00P C 0.4476(4) 0.93945(18) 0.8404(5) 0.0697(10) Uani 1 1 d . . . . .
H00X H 0.449190 0.974813 0.902138 0.084 Uiso 1 1 calc R U . . .
C00Q C 0.6428(6) 0.4754(2) 0.4204(7) 0.1045(17) Uani 1 1 d . . . . .
H00Y H 0.569852 0.457401 0.334096 0.157 Uiso 1 1 calc R U . . .
H H 0.681068 0.441174 0.494993 0.157 Uiso 1 1 calc R U . . .
HA H 0.707143 0.491840 0.390233 0.157 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
C001 0.0404(13) 0.0379(14) 0.0389(13) 0.0056(11) 0.0180(11) 0.0032(10)
O002 0.103(2) 0.0469(14) 0.0878(19) -0.0033(13) 0.0368(16) 0.0198(13)
C003 0.0444(13) 0.0438(15) 0.0396(14) -0.0004(12) 0.0211(11) 0.0003(11)
C004 0.0385(12) 0.0361(13) 0.0386(13) 0.0014(11) 0.0158(11) 0.0010(10)
O005 0.0866(19) 0.0507(15) 0.149(3) -0.0334(17) 0.0562(19) -0.0175(13)
C006 0.0516(15) 0.0427(15) 0.0435(15) -0.0031(12) 0.0187(12) 0.0007(12)
C007 0.0426(14) 0.0411(14) 0.0420(15) 0.0016(12) 0.0179(12) 0.0047(11)
C008 0.0688(19) 0.0498(17) 0.061(2) 0.0158(15) 0.0285(16) 0.0155(15)
C009 0.081(2) 0.063(2) 0.098(3) 0.016(2) 0.066(2) 0.0055(18)
C00A 0.0494(16) 0.0401(15) 0.0590(18) 0.0011(13) 0.0242(14) 0.0025(12)
C00B 0.086(2) 0.062(2) 0.0491(18) 0.0140(16) 0.0336(17) 0.0080(18)
C00C 0.0573(16) 0.0442(16) 0.0498(15) 0.0088(13) 0.0300(13) 0.0065(13)
C00D 0.071(2) 0.064(2) 0.076(2) -0.0149(18) 0.0452(19) -0.0232(17)
C00E 0.0534(17) 0.065(2) 0.0549(18) -0.0062(15) 0.0326(15) -0.0074(14)
C00F 0.0471(15) 0.0495(16) 0.0518(17) -0.0003(13) 0.0241(13) 0.0062(13)
C00G 0.078(3) 0.059(2) 0.124(4) -0.003(2) 0.040(3) -0.0189(19)
C00H 0.0713(19) 0.0564(19) 0.0437(16) 0.0021(14) 0.0317(15) 0.0057(15)
C00I 0.0550(17) 0.0426(16) 0.066(2) -0.0047(14) 0.0286(15) 0.0006(13)
C00J 0.0582(18) 0.0392(17) 0.081(2) -0.0081(16) 0.0252(17) 0.0034(13)
C00K 0.0544(16) 0.0429(15) 0.0431(15) -0.0016(12) 0.0266(13) -0.0060(12)
C00L 0.080(2) 0.054(2) 0.073(2) -0.0158(17) 0.0477(19) -0.0024(17)
C00M 0.098(3) 0.069(2) 0.0502(19) -0.0060(17) 0.045(2) -0.001(2)
C00N 0.098(3) 0.067(2) 0.0449(17) 0.0109(16) 0.0365(18) 0.0134(19)
C00O 0.0616(19) 0.060(2) 0.069(2) -0.0104(17) 0.0363(17) 0.0089(16)
C00P 0.075(2) 0.051(2) 0.084(3) -0.0172(18) 0.036(2) 0.0091(17)
C00Q 0.137(4) 0.049(2) 0.146(5) -0.006(3) 0.078(4) 0.024(3)
_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
C001 C003 1.481(4) . ?
C001 C004 1.353(3) . ?
C001 C00C 1.555(4) . ?
O002 C00I 1.378(4) . ?
O002 C00Q 1.408(5) . ?
C003 C006 1.387(4) . ?
C003 C00H 1.395(4) . ?
C004 C007 1.485(4) . ?
C004 C00K 1.553(4) . ?
O005 C00G 1.397(5) . ?
O005 C00J 1.372(4) . ?
C006 H006 0.9300 . ?
C006 C00I 1.392(4) . ?
C007 C00A 1.392(4) . ?
C007 C00F 1.397(4) . ?
C008 H00A 0.9600 . ?
C008 H00B 0.9600 . ?
C008 H00C 0.9600 . ?
C008 C00C 1.521(4) . ?
C009 H00D 0.9600 . ?
C009 H00E 0.9600 . ?
C009 H00F 0.9600 . ?
C009 C00C 1.545(5) . ?
C00A H00G 0.9300 . ?
C00A C00J 1.391(4) . ?
C00B H00H 0.9600 . ?
C00B H00I 0.9600 . ?
C00B H00J 0.9600 . ?
C00B C00K 1.543(4) . ?
C00C C00N 1.549(5) . ?
C00D H00K 0.9600 . ?
C00D H00L 0.9600 . ?
C00D H00M 0.9600 . ?
C00D C00K 1.527(4) . ?
C00E H00N 0.9700 . ?
C00E H00O 0.9700 . ?
C00E C00F 1.485(4) . ?
C00E C00K 1.555(4) . ?
C00F C00O 1.386(4) . ?
C00G H00P 0.9600 . ?
C00G H00Q 0.9600 . ?
C00G H00R 0.9600 . ?
C00H C00M 1.370(5) . ?
C00H C00N 1.501(5) . ?
C00I C00L 1.380(5) . ?
C00J C00P 1.396(5) . ?
C00L H00S 0.9300 . ?
C00L C00M 1.391(5) . ?
C00M H00T 0.9300 . ?
C00N H00U 0.9700 . ?
C00N H00V 0.9700 . ?
C00O H00W 0.9300 . ?
C00O C00P 1.374(5) . ?
C00P H00X 0.9300 . ?
C00Q H00Y 0.9600 . ?
C00Q H 0.9600 . ?
C00Q HA 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
C003 C001 C00C 104.5(2) . . ?
C004 C001 C003 127.1(2) . . ?
C004 C001 C00C 128.1(2) . . ?
C00I O002 C00Q 118.3(3) . . ?
C006 C003 C001 129.8(3) . . ?
C006 C003 C00H 119.3(3) . . ?
C00H C003 C001 110.3(3) . . ?
C001 C004 C007 127.9(2) . . ?
C001 C004 C00K 127.3(2) . . ?
C007 C004 C00K 104.7(2) . . ?
C00J O005 C00G 118.3(3) . . ?
C003 C006 H006 120.0 . . ?
C003 C006 C00I 120.0(3) . . ?
C00I C006 H006 120.0 . . ?
C00A C007 C004 129.8(3) . . ?
C00A C007 C00F 120.1(3) . . ?
C00F C007 C004 109.4(2) . . ?
H00A C008 H00B 109.5 . . ?
H00A C008 H00C 109.5 . . ?
H00B C008 H00C 109.5 . . ?
C00C C008 H00A 109.5 . . ?
C00C C008 H00B 109.5 . . ?
C00C C008 H00C 109.5 . . ?
H00D C009 H00E 109.5 . . ?
H00D C009 H00F 109.5 . . ?
H00E C009 H00F 109.5 . . ?
C00C C009 H00D 109.5 . . ?
C00C C009 H00E 109.5 . . ?
C00C C009 H00F 109.5 . . ?
C007 C00A H00G 120.6 . . ?
C00J C00A C007 118.8(3) . . ?
C00J C00A H00G 120.6 . . ?
H00H C00B H00I 109.5 . . ?
H00H C00B H00J 109.5 . . ?
H00I C00B H00J 109.5 . . ?
C00K C00B H00H 109.5 . . ?
C00K C00B H00I 109.5 . . ?
C00K C00B H00J 109.5 . . ?
C008 C00C C001 115.6(2) . . ?
C008 C00C C009 110.5(3) . . ?
C008 C00C C00N 109.6(3) . . ?
C009 C00C C001 110.9(3) . . ?
C009 C00C C00N 109.1(3) . . ?
C00N C00C C001 100.7(2) . . ?
H00K C00D H00L 109.5 . . ?
H00K C00D H00M 109.5 . . ?
H00L C00D H00M 109.5 . . ?
C00K C00D H00K 109.5 . . ?
C00K C00D H00L 109.5 . . ?
C00K C00D H00M 109.5 . . ?
H00N C00E H00O 109.0 . . ?
C00F C00E H00N 110.9 . . ?
C00F C00E H00O 110.9 . . ?
C00F C00E C00K 104.1(2) . . ?
C00K C00E H00N 110.9 . . ?
C00K C00E H00O 110.9 . . ?
C007 C00F C00E 109.8(3) . . ?
C00O C00F C007 120.4(3) . . ?
C00O C00F C00E 129.6(3) . . ?
O005 C00G H00P 109.5 . . ?
O005 C00G H00Q 109.5 . . ?
O005 C00G H00R 109.5 . . ?
H00P C00G H00Q 109.5 . . ?
H00P C00G H00R 109.5 . . ?
H00Q C00G H00R 109.5 . . ?
C003 C00H C00N 108.7(3) . . ?
C00M C00H C003 120.4(3) . . ?
C00M C00H C00N 130.9(3) . . ?
O002 C00I C006 114.4(3) . . ?
O002 C00I C00L 125.3(3) . . ?
C00L C00I C006 120.3(3) . . ?
O005 C00J C00A 124.0(3) . . ?
O005 C00J C00P 115.4(3) . . ?
C00A C00J C00P 120.6(3) . . ?
C004 C00K C00E 100.8(2) . . ?
C00B C00K C004 110.4(2) . . ?
C00B C00K C00E 107.6(3) . . ?
C00D C00K C004 116.4(2) . . ?
C00D C00K C00B 111.5(3) . . ?
C00D C00K C00E 109.3(2) . . ?
C00I C00L H00S 120.3 . . ?
C00I C00L C00M 119.4(3) . . ?
C00M C00L H00S 120.3 . . ?
C00H C00M C00L 120.5(3) . . ?
C00H C00M H00T 119.7 . . ?
C00L C00M H00T 119.7 . . ?
C00C C00N H00U 110.9 . . ?
C00C C00N H00V 110.9 . . ?
C00H C00N C00C 104.1(3) . . ?
C00H C00N H00U 110.9 . . ?
C00H C00N H00V 110.9 . . ?
H00U C00N H00V 108.9 . . ?
C00F C00O H00W 120.2 . . ?
C00P C00O C00F 119.6(3) . . ?
C00P C00O H00W 120.2 . . ?
C00J C00P H00X 119.8 . . ?
C00O C00P C00J 120.3(3) . . ?
C00O C00P H00X 119.8 . . ?
O002 C00Q H00Y 109.5 . . ?
O002 C00Q H 109.5 . . ?
O002 C00Q HA 109.5 . . ?
H00Y C00Q H 109.5 . . ?
H00Y C00Q HA 109.5 . . ?
H C00Q HA 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
C001 C003 C006 C00I -172.7(3) . . . . ?
C001 C003 C00H C00M 175.5(3) . . . . ?
C001 C003 C00H C00N -2.9(4) . . . . ?
C001 C004 C007 C00A -33.4(4) . . . . ?
C001 C004 C007 C00F 156.3(3) . . . . ?
C001 C004 C00K C00B 101.7(3) . . . . ?
C001 C004 C00K C00D -26.7(4) . . . . ?
C001 C004 C00K C00E -144.7(3) . . . . ?
C001 C00C C00N C00H -32.8(3) . . . . ?
O002 C00I C00L C00M -179.1(3) . . . . ?
C003 C001 C004 C007 164.9(3) . . . . ?
C003 C001 C004 C00K -20.3(4) . . . . ?
C003 C001 C00C C008 149.1(3) . . . . ?
C003 C001 C00C C009 -84.2(3) . . . . ?
C003 C001 C00C C00N 31.2(3) . . . . ?
C003 C006 C00I O002 -179.4(3) . . . . ?
C003 C006 C00I C00L 0.2(5) . . . . ?
C003 C00H C00M C00L -2.2(5) . . . . ?
C003 C00H C00N C00C 23.3(4) . . . . ?
C004 C001 C003 C006 -34.0(5) . . . . ?
C004 C001 C003 C00H 155.2(3) . . . . ?
C004 C001 C00C C008 -24.7(4) . . . . ?
C004 C001 C00C C009 102.0(3) . . . . ?
C004 C001 C00C C00N -142.6(3) . . . . ?
C004 C007 C00A C00J -171.6(3) . . . . ?
C004 C007 C00F C00E -1.7(3) . . . . ?
C004 C007 C00F C00O 174.1(3) . . . . ?
O005 C00J C00P C00O -176.9(4) . . . . ?
C006 C003 C00H C00M 3.6(5) . . . . ?
C006 C003 C00H C00N -174.7(3) . . . . ?
C006 C00I C00L C00M 1.3(5) . . . . ?
C007 C004 C00K C00B -82.6(3) . . . . ?
C007 C004 C00K C00D 149.0(3) . . . . ?
C007 C004 C00K C00E 31.0(3) . . . . ?
C007 C00A C00J O005 178.5(3) . . . . ?
C007 C00A C00J C00P 0.0(5) . . . . ?
C007 C00F C00O C00P -0.9(5) . . . . ?
C008 C00C C00N C00H -155.0(3) . . . . ?
C009 C00C C00N C00H 83.9(3) . . . . ?
C00A C007 C00F C00E -173.1(3) . . . . ?
C00A C007 C00F C00O 2.7(4) . . . . ?
C00A C00J C00P C00O 1.8(5) . . . . ?
C00C C001 C003 C006 152.0(3) . . . . ?
C00C C001 C003 C00H -18.7(3) . . . . ?
C00C C001 C004 C007 -22.5(4) . . . . ?
C00C C001 C004 C00K 152.2(3) . . . . ?
C00E C00F C00O C00P 173.9(3) . . . . ?
C00F C007 C00A C00J -2.2(4) . . . . ?
C00F C00E C00K C004 -31.8(3) . . . . ?
C00F C00E C00K C00B 83.9(3) . . . . ?
C00F C00E C00K C00D -154.9(3) . . . . ?
C00F C00O C00P C00J -1.3(5) . . . . ?
C00G O005 C00J C00A -9.7(6) . . . . ?
C00G O005 C00J C00P 168.9(4) . . . . ?
C00H C003 C006 C00I -2.7(4) . . . . ?
C00I C00L C00M C00H -0.3(5) . . . . ?
C00K C004 C007 C00A 150.9(3) . . . . ?
C00K C004 C007 C00F -19.3(3) . . . . ?
C00K C00E C00F C007 21.9(3) . . . . ?
C00K C00E C00F C00O -153.3(3) . . . . ?
C00M C00H C00N C00C -154.8(4) . . . . ?
C00N C00H C00M C00L 175.8(4) . . . . ?
C00Q O002 C00I C006 -169.0(4) . . . . ?
C00Q O002 C00I C00L 11.3(5) . . . . ?
_shelx_res_file
;
TITL mo_CNS_JS_186_0m_a.res in Cc
mo_cns_js_186_0m_a.res
created by SHELXL-2018/3 at 16:38:44 on 18-Dec-2023
REM Old TITL mo_CNS_JS_186_0m in Cc
REM SHELXT solution in Cc
REM R1 0.153, Rweak 0.041, Alpha 0.006, Orientation as input
REM Flack x = 0.398 ( 1.067 ) from Parsons' quotients
REM Formula found by SHELXT: C25 O
CELL 0.71073 11.3612 20.0633 9.8621 90 116.079 90
ZERR 4 0.0039 0.0072 0.0039 0 0.016 0
LATT -7
SYMM +X,-Y,0.5+Z
SFAC C H O
UNIT 96 112 8
L.S. 10
PLAN 5
SIZE 0.139 0.156 0.355
TEMP 19.85
CONF
BOND $H
LIST 4
MORE -1
fmap 2
acta
OMIT 0 2 1
OMIT 0 2 -1
OMIT 0 0 -12
REM
REM
REM
WGHT 0.037100 0.811000
FVAR 1.16483
C001 1 0.447440 0.760029 0.446763 11.00000 0.04043 0.03794 =
0.03893 0.00563 0.01796 0.00322
O002 3 0.599411 0.528009 0.481574 11.00000 0.10281 0.04691 =
0.08779 -0.00335 0.03684 0.01976
C003 1 0.464492 0.694309 0.389431 11.00000 0.04436 0.04383 =
0.03961 -0.00038 0.02110 0.00035
C004 1 0.426529 0.771932 0.569450 11.00000 0.03852 0.03606 =
0.03859 0.00143 0.01580 0.00104
O005 3 0.611106 0.994413 0.800253 11.00000 0.08661 0.05074 =
0.14860 -0.03338 0.05621 -0.01753
C006 1 0.522975 0.636704 0.467808 11.00000 0.05162 0.04269 =
0.04345 -0.00307 0.01869 0.00071
AFIX 43
H006 2 0.549870 0.634358 0.571403 11.00000 -1.20000
AFIX 0
C007 1 0.438739 0.836235 0.649210 11.00000 0.04264 0.04114 =
0.04199 0.00163 0.01791 0.00469
C008 1 0.360089 0.872346 0.306156 11.00000 0.06879 0.04983 =
0.06111 0.01580 0.02847 0.01546
AFIX 137
H00A 2 0.277661 0.859584 0.303491 11.00000 -1.50000
H00B 2 0.345055 0.894368 0.213534 11.00000 -1.50000
H00C 2 0.404896 0.902081 0.389401 11.00000 -1.50000
AFIX 0
C009 1 0.583518 0.830370 0.352219 11.00000 0.08109 0.06259 =
0.09829 0.01557 0.06613 0.00547
AFIX 137
H00D 2 0.624928 0.855011 0.444791 11.00000 -1.50000
H00E 2 0.579131 0.857506 0.269951 11.00000 -1.50000
H00F 2 0.633492 0.790904 0.358682 11.00000 -1.50000
AFIX 0
C00A 1 0.524746 0.889052 0.671252 11.00000 0.04937 0.04006 =
0.05901 0.00108 0.02424 0.00253
AFIX 43
H00G 2 0.578689 0.889847 0.622580 11.00000 -1.20000
AFIX 0
C00B 1 0.487038 0.695008 0.795140 11.00000 0.08579 0.06246 =
0.04914 0.01395 0.03362 0.00802
AFIX 137
H00H 2 0.547770 0.671374 0.769200 11.00000 -1.50000
H00I 2 0.452654 0.665307 0.845245 11.00000 -1.50000
H00J 2 0.531233 0.731410 0.861113 11.00000 -1.50000
AFIX 0
C00C 1 0.443515 0.810561 0.325235 11.00000 0.05733 0.04415 =
0.04980 0.00885 0.02996 0.00653
C00D 1 0.286236 0.666086 0.553507 11.00000 0.07135 0.06352 =
0.07620 -0.01489 0.04516 -0.02322
AFIX 137
H00K 2 0.229597 0.683013 0.455145 11.00000 -1.50000
H00L 2 0.234301 0.648846 0.600401 11.00000 -1.50000
H00M 2 0.339862 0.631108 0.544155 11.00000 -1.50000
AFIX 0
C00E 1 0.290958 0.769746 0.698947 11.00000 0.05341 0.06505 =
0.05494 -0.00621 0.03256 -0.00740
AFIX 23
H00N 2 0.202339 0.773942 0.619528 11.00000 -1.20000
H00O 2 0.287397 0.753652 0.789817 11.00000 -1.20000
AFIX 0
C00F 1 0.361386 0.834389 0.726868 11.00000 0.04712 0.04949 =
0.05184 -0.00029 0.02412 0.00621
C00G 1 0.710210 0.993111 0.752787 11.00000 0.07849 0.05927 =
0.12414 -0.00350 0.03978 -0.01893
AFIX 137
H00P 2 0.671921 0.995434 0.644607 11.00000 -1.50000
H00Q 2 0.759295 0.952506 0.786159 11.00000 -1.50000
H00R 2 0.767529 1.030497 0.794973 11.00000 -1.50000
AFIX 0
C00H 1 0.429702 0.698011 0.235236 11.00000 0.07127 0.05640 =
0.04367 0.00208 0.03173 0.00574
C00I 1 0.541428 0.582376 0.391394 11.00000 0.05499 0.04255 =
0.06595 -0.00474 0.02860 0.00057
C00J 1 0.528543 0.940599 0.767360 11.00000 0.05820 0.03916 =
0.08145 -0.00807 0.02520 0.00342
C00K 1 0.373651 0.722228 0.650261 11.00000 0.05443 0.04292 =
0.04307 -0.00156 0.02659 -0.00603
C00L 1 0.502186 0.585569 0.237766 11.00000 0.07960 0.05448 =
0.07274 -0.01583 0.04772 -0.00243
AFIX 43
H00S 2 0.512963 0.548962 0.186461 11.00000 -1.20000
AFIX 0
C00M 1 0.446361 0.644030 0.160318 11.00000 0.09842 0.06946 =
0.05018 -0.00596 0.04536 -0.00122
AFIX 43
H00T 2 0.420138 0.646493 0.056864 11.00000 -1.20000
AFIX 0
C00N 1 0.380645 0.767051 0.181097 11.00000 0.09796 0.06722 =
0.04488 0.01095 0.03654 0.01343
AFIX 23
H00U 2 0.285770 0.768824 0.137930 11.00000 -1.20000
H00V 2 0.408340 0.781705 0.105881 11.00000 -1.20000
AFIX 0
C00O 1 0.365461 0.886325 0.821498 11.00000 0.06158 0.06042 =
0.06856 -0.01045 0.03635 0.00891
AFIX 43
H00W 2 0.312929 0.885227 0.871921 11.00000 -1.20000
AFIX 0
C00P 1 0.447565 0.939445 0.840382 11.00000 0.07545 0.05096 =
0.08372 -0.01716 0.03587 0.00914
AFIX 43
H00X 2 0.449190 0.974813 0.902138 11.00000 -1.20000
AFIX 0
C00Q 1 0.642822 0.475422 0.420353 11.00000 0.13653 0.04856 =
0.14574 -0.00557 0.07805 0.02383
AFIX 137
H00Y 2 0.569852 0.457401 0.334096 11.00000 -1.50000
H 2 0.681068 0.441174 0.494993 11.00000 -1.50000
HA 2 0.707143 0.491840 0.390233 11.00000 -1.50000
AFIX 0
HKLF 4
REM mo_CNS_JS_186_0m_a.res in Cc
REM wR2 = 0.1258, GooF = S = 1.026, Restrained GooF = 1.026 for all data
REM R1 = 0.0547 for 4051 Fo > 4sig(Fo) and 0.0843 for all 5625 data
REM 241 parameters refined using 2 restraints
END
WGHT 0.0371 0.8111
REM Highest difference peak 0.155, deepest hole -0.140, 1-sigma level 0.029
Q1 1 0.4203 0.7415 0.6238 11.00000 0.05 0.16
Q2 1 0.4481 0.7223 0.4357 11.00000 0.05 0.15
Q3 1 0.5364 0.6728 0.4223 11.00000 0.05 0.14
Q4 1 0.4485 0.7916 0.3998 11.00000 0.05 0.13
Q5 1 0.3885 0.7714 0.4776 11.00000 0.05 0.13
;
_shelx_res_checksum 92806
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# 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_mo_cnsjin_22_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2319369'
loop_
_audit_author_name
_audit_author_address
'Charlotte Stindt'
;University of Groningen
Netherlands
;
_audit_update_record
;
2023-12-18 deposited with the CCDC. 2024-03-27 downloaded from the CCDC.
;
_audit_creation_date 2023-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C22 H24 O2'
_chemical_formula_sum 'C22 H24 O2'
_chemical_formula_weight 320.41
_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'
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 monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
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 13.2599(18)
_cell_length_b 8.8008(13)
_cell_length_c 15.7527(19)
_cell_angle_alpha 90
_cell_angle_beta 110.535(5)
_cell_angle_gamma 90
_cell_volume 1721.5(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9972
_cell_measurement_temperature 293
_cell_measurement_theta_max 28.48
_cell_measurement_theta_min 2.69
_shelx_estimated_absorpt_T_max 0.985
_shelx_estimated_absorpt_T_min 0.969
_exptl_absorpt_coefficient_mu 0.077
_exptl_absorpt_correction_T_max 0.7460
_exptl_absorpt_correction_T_min 0.6782
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0872 before and 0.0726 after correction.
The Ratio of minimum to maximum transmission is 0.9091.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.236
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 688
_exptl_crystal_size_max 0.415
_exptl_crystal_size_mid 0.218
_exptl_crystal_size_min 0.19
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1109
_diffrn_reflns_av_unetI/netI 0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 91760
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.583
_diffrn_reflns_theta_min 3.398
_diffrn_ambient_temperature 293
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_source_current 30.0
_diffrn_source_power 1.5
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3263
_reflns_number_total 4809
_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 'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max 0.263
_refine_diff_density_min -0.186
_refine_diff_density_rms 0.037
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 221
_refine_ls_number_reflns 4809
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0971
_refine_ls_R_factor_gt 0.0612
_refine_ls_restrained_S_all 1.061
_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^)+(0.0391P)^2^+0.8833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1238
_refine_ls_wR_factor_ref 0.1476
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C004(H00A,H00B), C009(H00F,H00G), C00H(H00L,H00M), C00M(H00Q,H00R)
2.b Aromatic/amide H refined with riding coordinates:
C00F(H00K), C00I(H00N), C00J(H00O), C00L(H00P)
2.c Idealised Me refined as rotating group:
C007(H00C,H00D,H00E), C00A(H00H,H00I,H00J), C00N(H00S,H00T,H00U), C00O(H00V,
H00W,H00X)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary iterative
_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
O001 O 0.56875(10) 0.21034(18) 0.59770(9) 0.0552(4) Uani 1 1 d . . . . .
O002 O -0.04075(11) 0.24193(16) -0.02610(8) 0.0542(4) Uani 1 1 d . . . . .
C003 C 0.21123(12) 0.31218(18) 0.28786(10) 0.0333(3) Uani 1 1 d . . . . .
C004 C 0.17975(13) 0.3497(2) 0.36972(11) 0.0386(4) Uani 1 1 d . . . . .
H00A H 0.239370 0.395460 0.417809 0.046 Uiso 1 1 calc R U . . .
H00B H 0.156298 0.259446 0.392924 0.046 Uiso 1 1 calc R U . . .
C005 C 0.08148(12) 0.26138(18) 0.12243(10) 0.0340(3) Uani 1 1 d . . . . .
C006 C 0.31285(13) 0.30706(19) 0.28750(10) 0.0351(3) Uani 1 1 d . . . . .
C007 C 0.14529(14) 0.1387(2) 0.09764(12) 0.0433(4) Uani 1 1 d . . . . .
H00C H 0.183112 0.181360 0.061290 0.065 Uiso 1 1 calc R U . . .
H00D H 0.097346 0.060626 0.063954 0.065 Uiso 1 1 calc R U . . .
H00E H 0.196123 0.095976 0.151867 0.065 Uiso 1 1 calc R U . . .
C008 C 0.11069(12) 0.32576(17) 0.20836(10) 0.0323(3) Uani 1 1 d . . . . .
C009 C 0.34460(14) 0.3366(2) 0.20468(12) 0.0438(4) Uani 1 1 d . . . . .
H00F H 0.287335 0.388055 0.157324 0.053 Uiso 1 1 calc R U . . .
H00G H 0.361798 0.242478 0.180698 0.053 Uiso 1 1 calc R U . . .
C00A C 0.37064(14) 0.1389(2) 0.47896(12) 0.0448(4) Uani 1 1 d . . . . .
H00H H 0.340065 0.191427 0.517581 0.067 Uiso 1 1 calc R U . . .
H00I H 0.412019 0.053811 0.510977 0.067 Uiso 1 1 calc R U . . .
H00J H 0.313941 0.103443 0.425823 0.067 Uiso 1 1 calc R U . . .
C00B C 0.41514(12) 0.31045(19) 0.36582(11) 0.0355(3) Uani 1 1 d . . . . .
C00C C 0.03869(13) 0.41864(18) 0.23287(12) 0.0375(4) Uani 1 1 d . . . . .
C00D C -0.01780(14) 0.30552(19) 0.05811(11) 0.0405(4) Uani 1 1 d . . . . .
C00E C 0.44244(13) 0.24509(19) 0.45158(11) 0.0364(3) Uani 1 1 d . . . . .
C00F C -0.08706(15) 0.4026(2) 0.08094(13) 0.0483(4) Uani 1 1 d . . . . .
H00K H -0.151939 0.431726 0.037164 0.058 Uiso 1 1 calc R U . . .
C00G C 0.49199(13) 0.3900(2) 0.33988(12) 0.0418(4) Uani 1 1 d . . . . .
C00H C 0.08645(14) 0.4632(2) 0.33118(12) 0.0463(4) Uani 1 1 d . . . . .
H00L H 0.034106 0.452941 0.361075 0.056 Uiso 1 1 calc R U . . .
H00M H 0.112667 0.567032 0.337734 0.056 Uiso 1 1 calc R U . . .
C00I C 0.59474(15) 0.4101(2) 0.40118(14) 0.0508(5) Uani 1 1 d . . . . .
H00N H 0.645674 0.462228 0.384190 0.061 Uiso 1 1 calc R U . . .
C00J C -0.05925(14) 0.4562(2) 0.16922(13) 0.0477(4) Uani 1 1 d . . . . .
H00O H -0.106926 0.517403 0.185196 0.057 Uiso 1 1 calc R U . . .
C00K C 0.54713(14) 0.2724(2) 0.51309(12) 0.0424(4) Uani 1 1 d . . . . .
C00L C 0.62199(15) 0.3526(2) 0.48806(14) 0.0506(5) Uani 1 1 d . . . . .
H00P H 0.690932 0.368007 0.529832 0.061 Uiso 1 1 calc R U . . .
C00M C 0.44475(15) 0.4388(2) 0.24245(13) 0.0500(5) Uani 1 1 d . . . . .
H00Q H 0.494815 0.421299 0.210994 0.060 Uiso 1 1 calc R U . . .
H00R H 0.424953 0.545408 0.237567 0.060 Uiso 1 1 calc R U . . .
C00N C -0.13137(17) 0.2961(3) -0.09838(14) 0.0635(6) Uani 1 1 d . . . . .
H00S H -0.134043 0.248085 -0.153848 0.095 Uiso 1 1 calc R U . . .
H00T H -0.125608 0.404130 -0.103825 0.095 Uiso 1 1 calc R U . . .
H00U H -0.195869 0.272811 -0.086442 0.095 Uiso 1 1 calc R U . . .
C00O C 0.67266(17) 0.2335(3) 0.66314(15) 0.0689(7) Uani 1 1 d . . . . .
H00V H 0.725595 0.187478 0.642545 0.103 Uiso 1 1 calc R U . . .
H00W H 0.676216 0.188168 0.719554 0.103 Uiso 1 1 calc R U . . .
H00X H 0.686599 0.340482 0.671673 0.103 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
O001 0.0430(7) 0.0720(10) 0.0426(7) -0.0007(6) 0.0048(6) -0.0057(7)
O002 0.0575(8) 0.0547(8) 0.0387(7) -0.0005(6) 0.0023(6) 0.0046(7)
C003 0.0362(8) 0.0322(8) 0.0345(8) -0.0025(6) 0.0162(6) -0.0009(6)
C004 0.0413(9) 0.0418(9) 0.0385(8) -0.0079(7) 0.0213(7) -0.0044(7)
C005 0.0346(8) 0.0334(8) 0.0352(8) 0.0025(6) 0.0136(6) -0.0002(6)
C006 0.0360(8) 0.0376(8) 0.0353(8) -0.0029(6) 0.0170(6) -0.0004(7)
C007 0.0467(10) 0.0449(10) 0.0398(9) -0.0057(7) 0.0170(8) 0.0042(8)
C008 0.0322(7) 0.0304(7) 0.0376(8) 0.0008(6) 0.0165(6) -0.0003(6)
C009 0.0416(9) 0.0553(11) 0.0407(9) -0.0003(8) 0.0220(8) 0.0007(8)
C00A 0.0413(9) 0.0507(10) 0.0430(9) 0.0018(8) 0.0154(8) -0.0033(8)
C00B 0.0327(8) 0.0370(8) 0.0410(8) -0.0066(7) 0.0180(7) -0.0019(6)
C00C 0.0370(8) 0.0331(8) 0.0476(9) -0.0014(7) 0.0215(7) 0.0009(7)
C00D 0.0426(9) 0.0362(8) 0.0400(9) 0.0045(7) 0.0112(7) -0.0013(7)
C00E 0.0331(8) 0.0378(8) 0.0401(8) -0.0071(7) 0.0152(7) -0.0013(7)
C00F 0.0381(9) 0.0448(10) 0.0571(11) 0.0086(8) 0.0105(8) 0.0064(8)
C00G 0.0370(9) 0.0428(9) 0.0506(10) -0.0033(8) 0.0216(8) -0.0039(7)
C00H 0.0450(10) 0.0462(10) 0.0557(11) -0.0119(8) 0.0278(9) 0.0006(8)
C00I 0.0400(10) 0.0505(11) 0.0663(12) -0.0044(9) 0.0241(9) -0.0116(8)
C00J 0.0419(10) 0.0417(10) 0.0631(12) 0.0024(8) 0.0230(9) 0.0092(8)
C00K 0.0374(9) 0.0450(10) 0.0424(9) -0.0085(7) 0.0109(7) -0.0008(7)
C00L 0.0355(9) 0.0519(11) 0.0598(12) -0.0106(9) 0.0110(8) -0.0101(8)
C00M 0.0464(10) 0.0579(12) 0.0552(11) 0.0049(9) 0.0297(9) -0.0037(9)
C00N 0.0584(13) 0.0690(14) 0.0469(11) 0.0092(10) -0.0020(9) -0.0032(11)
C00O 0.0469(12) 0.0977(19) 0.0507(12) -0.0050(12) 0.0027(9) -0.0017(12)
_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
O001 C00K 1.374(2) . ?
O001 C00O 1.416(2) . ?
O002 C00D 1.372(2) . ?
O002 C00N 1.417(2) . ?
C003 C004 1.524(2) . ?
C003 C006 1.350(2) . ?
C003 C008 1.479(2) . ?
C004 H00A 0.9700 . ?
C004 H00B 0.9700 . ?
C004 C00H 1.540(2) . ?
C005 C007 1.505(2) . ?
C005 C008 1.391(2) . ?
C005 C00D 1.405(2) . ?
C006 C009 1.527(2) . ?
C006 C00B 1.479(2) . ?
C007 H00C 0.9600 . ?
C007 H00D 0.9600 . ?
C007 H00E 0.9600 . ?
C008 C00C 1.410(2) . ?
C009 H00F 0.9700 . ?
C009 H00G 0.9700 . ?
C009 C00M 1.540(3) . ?
C00A H00H 0.9600 . ?
C00A H00I 0.9600 . ?
C00A H00J 0.9600 . ?
C00A C00E 1.501(2) . ?
C00B C00E 1.394(2) . ?
C00B C00G 1.410(2) . ?
C00C C00H 1.505(2) . ?
C00C C00J 1.374(2) . ?
C00D C00F 1.391(3) . ?
C00E C00K 1.407(2) . ?
C00F H00K 0.9300 . ?
C00F C00J 1.390(3) . ?
C00G C00I 1.377(2) . ?
C00G C00M 1.503(3) . ?
C00H H00L 0.9700 . ?
C00H H00M 0.9700 . ?
C00I H00N 0.9300 . ?
C00I C00L 1.383(3) . ?
C00J H00O 0.9300 . ?
C00K C00L 1.384(3) . ?
C00L H00P 0.9300 . ?
C00M H00Q 0.9700 . ?
C00M H00R 0.9700 . ?
C00N H00S 0.9600 . ?
C00N H00T 0.9600 . ?
C00N H00U 0.9600 . ?
C00O H00V 0.9600 . ?
C00O H00W 0.9600 . ?
C00O H00X 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
C00K O001 C00O 117.87(16) . . ?
C00D O002 C00N 118.53(16) . . ?
C006 C003 C004 125.49(14) . . ?
C006 C003 C008 127.12(14) . . ?
C008 C003 C004 105.41(13) . . ?
C003 C004 H00A 111.1 . . ?
C003 C004 H00B 111.1 . . ?
C003 C004 C00H 103.16(13) . . ?
H00A C004 H00B 109.1 . . ?
C00H C004 H00A 111.1 . . ?
C00H C004 H00B 111.1 . . ?
C008 C005 C007 123.68(14) . . ?
C008 C005 C00D 117.36(15) . . ?
C00D C005 C007 118.74(14) . . ?
C003 C006 C009 124.92(15) . . ?
C003 C006 C00B 128.33(14) . . ?
C00B C006 C009 105.20(13) . . ?
C005 C007 H00C 109.5 . . ?
C005 C007 H00D 109.5 . . ?
C005 C007 H00E 109.5 . . ?
H00C C007 H00D 109.5 . . ?
H00C C007 H00E 109.5 . . ?
H00D C007 H00E 109.5 . . ?
C005 C008 C003 130.64(14) . . ?
C005 C008 C00C 121.24(15) . . ?
C00C C008 C003 108.10(13) . . ?
C006 C009 H00F 111.1 . . ?
C006 C009 H00G 111.1 . . ?
C006 C009 C00M 103.18(14) . . ?
H00F C009 H00G 109.1 . . ?
C00M C009 H00F 111.1 . . ?
C00M C009 H00G 111.1 . . ?
H00H C00A H00I 109.5 . . ?
H00H C00A H00J 109.5 . . ?
H00I C00A H00J 109.5 . . ?
C00E C00A H00H 109.5 . . ?
C00E C00A H00I 109.5 . . ?
C00E C00A H00J 109.5 . . ?
C00E C00B C006 130.56(14) . . ?
C00E C00B C00G 121.16(15) . . ?
C00G C00B C006 108.22(14) . . ?
C008 C00C C00H 110.62(14) . . ?
C00J C00C C008 119.81(16) . . ?
C00J C00C C00H 129.57(15) . . ?
O002 C00D C005 114.73(15) . . ?
O002 C00D C00F 123.92(16) . . ?
C00F C00D C005 121.32(16) . . ?
C00B C00E C00A 124.05(15) . . ?
C00B C00E C00K 117.06(15) . . ?
C00K C00E C00A 118.71(15) . . ?
C00D C00F H00K 120.0 . . ?
C00J C00F C00D 119.96(17) . . ?
C00J C00F H00K 120.0 . . ?
C00B C00G C00M 110.69(15) . . ?
C00I C00G C00B 119.89(17) . . ?
C00I C00G C00M 129.41(16) . . ?
C004 C00H H00L 111.1 . . ?
C004 C00H H00M 111.1 . . ?
C00C C00H C004 103.08(13) . . ?
C00C C00H H00L 111.1 . . ?
C00C C00H H00M 111.1 . . ?
H00L C00H H00M 109.1 . . ?
C00G C00I H00N 120.1 . . ?
C00G C00I C00L 119.85(17) . . ?
C00L C00I H00N 120.1 . . ?
C00C C00J C00F 119.98(16) . . ?
C00C C00J H00O 120.0 . . ?
C00F C00J H00O 120.0 . . ?
O001 C00K C00E 114.82(15) . . ?
O001 C00K C00L 123.56(16) . . ?
C00L C00K C00E 121.61(17) . . ?
C00I C00L C00K 120.28(17) . . ?
C00I C00L H00P 119.9 . . ?
C00K C00L H00P 119.9 . . ?
C009 C00M H00Q 111.2 . . ?
C009 C00M H00R 111.2 . . ?
C00G C00M C009 102.81(14) . . ?
C00G C00M H00Q 111.2 . . ?
C00G C00M H00R 111.2 . . ?
H00Q C00M H00R 109.1 . . ?
O002 C00N H00S 109.5 . . ?
O002 C00N H00T 109.5 . . ?
O002 C00N H00U 109.5 . . ?
H00S C00N H00T 109.5 . . ?
H00S C00N H00U 109.5 . . ?
H00T C00N H00U 109.5 . . ?
O001 C00O H00V 109.5 . . ?
O001 C00O H00W 109.5 . . ?
O001 C00O H00X 109.5 . . ?
H00V C00O H00W 109.5 . . ?
H00V C00O H00X 109.5 . . ?
H00W C00O H00X 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
O001 C00K C00L C00I 179.15(18) . . . . ?
O002 C00D C00F C00J 176.99(17) . . . . ?
C003 C004 C00H C00C 28.04(16) . . . . ?
C003 C006 C009 C00M 136.05(18) . . . . ?
C003 C006 C00B C00E 37.4(3) . . . . ?
C003 C006 C00B C00G -145.56(18) . . . . ?
C003 C008 C00C C00H -3.12(18) . . . . ?
C003 C008 C00C C00J 176.50(15) . . . . ?
C004 C003 C006 C009 -152.63(17) . . . . ?
C004 C003 C006 C00B 11.0(3) . . . . ?
C004 C003 C008 C005 -156.89(16) . . . . ?
C004 C003 C008 C00C 21.50(17) . . . . ?
C005 C008 C00C C00H 175.45(15) . . . . ?
C005 C008 C00C C00J -4.9(2) . . . . ?
C005 C00D C00F C00J -1.0(3) . . . . ?
C006 C003 C004 C00H 134.22(17) . . . . ?
C006 C003 C008 C005 38.6(3) . . . . ?
C006 C003 C008 C00C -143.05(17) . . . . ?
C006 C009 C00M C00G 28.96(18) . . . . ?
C006 C00B C00E C00A 6.6(3) . . . . ?
C006 C00B C00E C00K -178.42(16) . . . . ?
C006 C00B C00G C00I 179.67(16) . . . . ?
C006 C00B C00G C00M -1.6(2) . . . . ?
C007 C005 C008 C003 10.3(3) . . . . ?
C007 C005 C008 C00C -167.89(15) . . . . ?
C007 C005 C00D O002 -7.0(2) . . . . ?
C007 C005 C00D C00F 171.09(16) . . . . ?
C008 C003 C004 C00H -30.66(16) . . . . ?
C008 C003 C006 C009 9.0(3) . . . . ?
C008 C003 C006 C00B 172.65(15) . . . . ?
C008 C005 C00D O002 178.10(14) . . . . ?
C008 C005 C00D C00F -3.8(2) . . . . ?
C008 C00C C00H C004 -16.15(18) . . . . ?
C008 C00C C00J C00F 0.0(3) . . . . ?
C009 C006 C00B C00E -156.39(17) . . . . ?
C009 C006 C00B C00G 20.61(18) . . . . ?
C00A C00E C00K O001 -7.1(2) . . . . ?
C00A C00E C00K C00L 171.39(17) . . . . ?
C00B C006 C009 C00M -30.73(18) . . . . ?
C00B C00E C00K O001 177.66(15) . . . . ?
C00B C00E C00K C00L -3.9(3) . . . . ?
C00B C00G C00I C00L -0.2(3) . . . . ?
C00B C00G C00M C009 -17.7(2) . . . . ?
C00D C005 C008 C003 -175.10(15) . . . . ?
C00D C005 C008 C00C 6.7(2) . . . . ?
C00D C00F C00J C00C 2.9(3) . . . . ?
C00E C00B C00G C00I -3.0(3) . . . . ?
C00E C00B C00G C00M 175.71(15) . . . . ?
C00E C00K C00L C00I 0.8(3) . . . . ?
C00G C00B C00E C00A -170.04(16) . . . . ?
C00G C00B C00E C00K 4.9(2) . . . . ?
C00G C00I C00L C00K 1.3(3) . . . . ?
C00H C00C C00J C00F 179.52(18) . . . . ?
C00I C00G C00M C009 160.88(19) . . . . ?
C00J C00C C00H C004 164.28(18) . . . . ?
C00M C00G C00I C00L -178.67(19) . . . . ?
C00N O002 C00D C005 -171.14(16) . . . . ?
C00N O002 C00D C00F 10.8(3) . . . . ?
C00O O001 C00K C00E -179.94(17) . . . . ?
C00O O001 C00K C00L 1.6(3) . . . . ?
_shelx_res_file
;
TITL mo_CNSJIN_22_0ma_a.res in P2(1)/c
mo_cnsjin_22_0ma_a.res
created by SHELXL-2018/3 at 16:38:29 on 18-Dec-2023
REM Old TITL mo_CNSJIN_22_0ma in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.191, Rweak 0.005, Alpha 0.040, Orientation as input
REM Formula found by SHELXT: C22 O2
CELL 0.71073 13.2599 8.8008 15.7527 90 110.535 90
ZERR 4 0.0018 0.0013 0.0019 0 0.005 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H O
UNIT 88 96 8
L.S. 10
PLAN 1
SIZE 0.19 0.218 0.415
TEMP 19.85
CONF
LIST 4
MORE -1
BOND $H
fmap 2
acta
OMIT 2 0 0
OMIT -2 0 2
OMIT -1 1 1
OMIT -1 0 2
OMIT 1 1 0
REM
REM
REM
WGHT 0.039100 0.883300
FVAR 1.30422
O001 3 0.568752 0.210338 0.597704 11.00000 0.04300 0.07197 =
0.04257 -0.00073 0.00477 -0.00572
O002 3 -0.040747 0.241928 -0.026098 11.00000 0.05753 0.05466 =
0.03868 -0.00051 0.00230 0.00459
C003 1 0.211234 0.312180 0.287857 11.00000 0.03618 0.03218 =
0.03453 -0.00250 0.01615 -0.00092
C004 1 0.179748 0.349697 0.369721 11.00000 0.04131 0.04184 =
0.03853 -0.00789 0.02134 -0.00443
AFIX 23
H00A 2 0.239370 0.395460 0.417809 11.00000 -1.20000
H00B 2 0.156298 0.259446 0.392924 11.00000 -1.20000
AFIX 0
C005 1 0.081481 0.261378 0.122433 11.00000 0.03460 0.03338 =
0.03523 0.00251 0.01361 -0.00020
C006 1 0.312850 0.307059 0.287498 11.00000 0.03602 0.03759 =
0.03527 -0.00287 0.01697 -0.00037
C007 1 0.145293 0.138730 0.097641 11.00000 0.04671 0.04495 =
0.03982 -0.00566 0.01699 0.00421
AFIX 137
H00C 2 0.183112 0.181360 0.061290 11.00000 -1.50000
H00D 2 0.097346 0.060626 0.063954 11.00000 -1.50000
H00E 2 0.196123 0.095976 0.151867 11.00000 -1.50000
AFIX 0
C008 1 0.110686 0.325765 0.208355 11.00000 0.03225 0.03038 =
0.03758 0.00081 0.01648 -0.00030
C009 1 0.344596 0.336570 0.204678 11.00000 0.04164 0.05527 =
0.04069 -0.00031 0.02204 0.00075
AFIX 23
H00F 2 0.287335 0.388055 0.157324 11.00000 -1.20000
H00G 2 0.361798 0.242478 0.180698 11.00000 -1.20000
AFIX 0
C00A 1 0.370643 0.138867 0.478958 11.00000 0.04132 0.05068 =
0.04301 0.00177 0.01538 -0.00327
AFIX 137
H00H 2 0.340065 0.191427 0.517581 11.00000 -1.50000
H00I 2 0.412019 0.053811 0.510977 11.00000 -1.50000
H00J 2 0.313941 0.103443 0.425823 11.00000 -1.50000
AFIX 0
C00B 1 0.415138 0.310452 0.365825 11.00000 0.03270 0.03697 =
0.04102 -0.00664 0.01805 -0.00193
C00C 1 0.038694 0.418641 0.232873 11.00000 0.03705 0.03310 =
0.04759 -0.00142 0.02151 0.00087
C00D 1 -0.017801 0.305524 0.058108 11.00000 0.04256 0.03622 =
0.03998 0.00447 0.01118 -0.00131
C00E 1 0.442437 0.245091 0.451581 11.00000 0.03315 0.03782 =
0.04011 -0.00712 0.01519 -0.00125
C00F 1 -0.087063 0.402639 0.080939 11.00000 0.03813 0.04481 =
0.05711 0.00863 0.01053 0.00636
AFIX 43
H00K 2 -0.151939 0.431726 0.037164 11.00000 -1.20000
AFIX 0
C00G 1 0.491987 0.390022 0.339880 11.00000 0.03701 0.04276 =
0.05061 -0.00329 0.02155 -0.00386
C00H 1 0.086446 0.463232 0.331182 11.00000 0.04499 0.04621 =
0.05574 -0.01185 0.02783 0.00056
AFIX 23
H00L 2 0.034106 0.452941 0.361075 11.00000 -1.20000
H00M 2 0.112667 0.567032 0.337734 11.00000 -1.20000
AFIX 0
C00I 1 0.594741 0.410123 0.401184 11.00000 0.03998 0.05046 =
0.06629 -0.00436 0.02411 -0.01160
AFIX 43
H00N 2 0.645674 0.462228 0.384190 11.00000 -1.20000
AFIX 0
C00J 1 -0.059249 0.456183 0.169222 11.00000 0.04193 0.04166 =
0.06314 0.00238 0.02299 0.00921
AFIX 43
H00O 2 -0.106926 0.517403 0.185196 11.00000 -1.20000
AFIX 0
C00K 1 0.547128 0.272389 0.513086 11.00000 0.03740 0.04505 =
0.04240 -0.00849 0.01095 -0.00085
C00L 1 0.621994 0.352650 0.488056 11.00000 0.03547 0.05194 =
0.05978 -0.01062 0.01105 -0.01009
AFIX 43
H00P 2 0.690932 0.368007 0.529832 11.00000 -1.20000
AFIX 0
C00M 1 0.444748 0.438801 0.242455 11.00000 0.04637 0.05788 =
0.05517 0.00488 0.02972 -0.00372
AFIX 23
H00Q 2 0.494815 0.421299 0.210994 11.00000 -1.20000
H00R 2 0.424953 0.545408 0.237567 11.00000 -1.20000
AFIX 0
C00N 1 -0.131374 0.296107 -0.098382 11.00000 0.05837 0.06900 =
0.04693 0.00917 -0.00196 -0.00323
AFIX 137
H00S 2 -0.134043 0.248085 -0.153848 11.00000 -1.50000
H00T 2 -0.125608 0.404130 -0.103825 11.00000 -1.50000
H00U 2 -0.195869 0.272811 -0.086442 11.00000 -1.50000
AFIX 0
C00O 1 0.672660 0.233481 0.663140 11.00000 0.04686 0.09772 =
0.05069 -0.00497 0.00265 -0.00168
AFIX 137
H00V 2 0.725595 0.187478 0.642545 11.00000 -1.50000
H00W 2 0.676216 0.188168 0.719554 11.00000 -1.50000
H00X 2 0.686599 0.340482 0.671673 11.00000 -1.50000
AFIX 0
HKLF 4
REM mo_CNSJIN_22_0ma_a.res in P2(1)/c
REM wR2 = 0.1476, GooF = S = 1.061, Restrained GooF = 1.061 for all data
REM R1 = 0.0612 for 3263 Fo > 4sig(Fo) and 0.0971 for all 4809 data
REM 221 parameters refined using 0 restraints
END
WGHT 0.0391 0.8837
REM Highest difference peak 0.263, deepest hole -0.186, 1-sigma level 0.037
Q1 1 0.0312 0.2746 0.0980 11.00000 0.05 0.26
;
_shelx_res_checksum 78918
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# 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_mo_cns_jin_12_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2319370'
loop_
_audit_author_name
_audit_author_address
'Charlotte Stindt'
;University of Groningen
Netherlands
;
_audit_update_record
;
2023-12-18 deposited with the CCDC. 2024-03-27 downloaded from the CCDC.
;
_audit_creation_date 2023-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C26 H28 O4'
_chemical_formula_sum 'C26 H28 O4'
_chemical_formula_weight 404.48
_chemical_absolute_configuration ?
_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'
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 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a 9.6167(8)
_cell_length_b 12.0209(10)
_cell_length_c 18.8367(16)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2177.5(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9993
_cell_measurement_temperature 293
_cell_measurement_theta_max 23.39
_cell_measurement_theta_min 2.71
_shelx_estimated_absorpt_T_max 0.990
_shelx_estimated_absorpt_T_min 0.986
_exptl_absorpt_coefficient_mu 0.082
_exptl_absorpt_correction_T_max 0.5809
_exptl_absorpt_correction_T_min 0.5190
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1340 before and 0.1164 after correction.
The Ratio of minimum to maximum transmission is 0.8934.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.234
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 864
_exptl_crystal_size_max 0.175
_exptl_crystal_size_mid 0.137
_exptl_crystal_size_min 0.117
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1663
_diffrn_reflns_av_unetI/netI 0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 111523
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.584
_diffrn_reflns_theta_min 2.378
_diffrn_ambient_temperature 293
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_source_current 30.0
_diffrn_source_power 1.5
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.780
_reflns_Friedel_fraction_full 0.999
_reflns_Friedel_fraction_max 0.999
_reflns_number_gt 4704
_reflns_number_total 6111
_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 'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max 0.159
_refine_diff_density_min -0.192
_refine_diff_density_rms 0.040
_refine_ls_abs_structure_details
;
Flack x determined using 1603 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.3(7)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.025
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 277
_refine_ls_number_reflns 6111
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0766
_refine_ls_R_factor_gt 0.0545
_refine_ls_restrained_S_all 1.025
_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^)+(0.0446P)^2^+0.5205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1163
_refine_ls_wR_factor_ref 0.1297
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C006(H00A,H00B), C00T(H00W,H00X)
2.b Aromatic/amide H refined with riding coordinates:
C005(H005), C00A(H00F), C00F(H00J), C00I(H00N), C00K(H00O), C00N(H00P)
2.c Idealised Me refined as rotating group:
C009(H00C,H00D,H00E), C00B(H00G,H00H,H00I), C00G(H00K,H00L,H00M), C00P(H00Q,
H00R,H00S), C00S(H00T,H00U,H00V), C00U(H00Y,H,HA)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary iterative
_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
O001 O 0.4764(2) 0.25546(17) 0.70645(11) 0.0550(6) Uani 1 1 d . . . . .
O002 O 0.4247(3) 0.78454(17) 0.29101(10) 0.0547(5) Uani 1 1 d . . . . .
O003 O 0.3497(4) 1.0754(2) 0.38164(15) 0.0851(9) Uani 1 1 d . . . . .
O004 O 0.2068(3) 0.01296(19) 0.66711(15) 0.0787(8) Uani 1 1 d . . . . .
C005 C 0.3208(3) 0.8810(2) 0.46544(15) 0.0414(6) Uani 1 1 d . . . . .
H005 H 0.304777 0.948393 0.488275 0.050 Uiso 1 1 calc R U . . .
C006 C 0.2713(3) 0.7624(2) 0.57816(14) 0.0439(6) Uani 1 1 d . . . . .
H00A H 0.171449 0.762493 0.585333 0.053 Uiso 1 1 calc R U . . .
H00B H 0.312920 0.818488 0.608468 0.053 Uiso 1 1 calc R U . . .
C007 C 0.3339(3) 0.6456(2) 0.59364(13) 0.0356(5) Uani 1 1 d . . . . .
C008 C 0.3064(3) 0.7826(2) 0.50234(14) 0.0382(5) Uani 1 1 d . . . . .
C009 C 0.4885(3) 0.6600(2) 0.61106(15) 0.0432(6) Uani 1 1 d . . . . .
H00C H 0.531634 0.705376 0.575349 0.065 Uiso 1 1 calc R U . . .
H00D H 0.532782 0.588455 0.612208 0.065 Uiso 1 1 calc R U . . .
H00E H 0.498022 0.695276 0.656529 0.065 Uiso 1 1 calc R U . . .
C00A C 0.3734(4) 0.9857(2) 0.35573(19) 0.0556(8) Uani 1 1 d . . . . .
H00F H 0.402413 0.983243 0.308659 0.067 Uiso 1 1 calc R U . . .
C00B C 0.2540(3) 0.5948(3) 0.65582(16) 0.0475(7) Uani 1 1 d . . . . .
H00G H 0.237391 0.650971 0.691057 0.071 Uiso 1 1 calc R U . . .
H00H H 0.307738 0.535629 0.676276 0.071 Uiso 1 1 calc R U . . .
H00I H 0.166806 0.566006 0.639213 0.071 Uiso 1 1 calc R U . . .
C00C C 0.2852(3) 0.4809(2) 0.50616(13) 0.0357(5) Uani 1 1 d . . . . .
C00D C 0.3871(3) 0.2757(2) 0.65139(14) 0.0404(6) Uani 1 1 d . . . . .
C00E C 0.3163(2) 0.5891(2) 0.51990(13) 0.0338(5) Uani 1 1 d . . . . .
C00F C 0.3923(3) 0.3726(2) 0.61159(13) 0.0378(5) Uani 1 1 d . . . . .
H00J H 0.458186 0.427044 0.621568 0.045 Uiso 1 1 calc R U . . .
C00G C 0.3211(4) 0.3765(3) 0.38986(16) 0.0564(8) Uani 1 1 d . . . . .
H00K H 0.386156 0.431735 0.374041 0.085 Uiso 1 1 calc R U . . .
H00L H 0.274282 0.344962 0.349592 0.085 Uiso 1 1 calc R U . . .
H00M H 0.369799 0.318926 0.414954 0.085 Uiso 1 1 calc R U . . .
C00H C 0.2909(3) 0.1919(2) 0.63545(15) 0.0431(6) Uani 1 1 d . . . . .
C00I C 0.3722(3) 0.6783(2) 0.39737(14) 0.0384(6) Uani 1 1 d . . . . .
H00N H 0.392225 0.610941 0.375321 0.046 Uiso 1 1 calc R U . . .
C00J C 0.3591(3) 0.8800(2) 0.39418(15) 0.0414(6) Uani 1 1 d . . . . .
C00K C 0.2031(3) 0.2054(2) 0.57732(16) 0.0465(6) Uani 1 1 d . . . . .
H00O H 0.141655 0.148906 0.565032 0.056 Uiso 1 1 calc R U . . .
C00L C 0.3289(2) 0.6806(2) 0.46785(13) 0.0336(5) Uani 1 1 d . . . . .
C00M C 0.2975(3) 0.3875(2) 0.55649(14) 0.0371(5) Uani 1 1 d . . . . .
C00N C 0.2810(4) 0.0914(2) 0.67952(18) 0.0558(8) Uani 1 1 d . . . . .
H00P H 0.336203 0.087998 0.720011 0.067 Uiso 1 1 calc R U . . .
C00O C 0.2139(3) 0.4306(2) 0.43945(15) 0.0440(6) Uani 1 1 d . . . . .
C00P C 0.1166(3) 0.5077(3) 0.39834(18) 0.0566(8) Uani 1 1 d . . . . .
H00Q H 0.058222 0.547281 0.431071 0.085 Uiso 1 1 calc R U . . .
H00R H 0.059830 0.464454 0.366793 0.085 Uiso 1 1 calc R U . . .
H00S H 0.170613 0.559860 0.371326 0.085 Uiso 1 1 calc R U . . .
C00Q C 0.2065(3) 0.3017(2) 0.53792(15) 0.0440(6) Uani 1 1 d . . . . .
C00R C 0.3852(3) 0.7780(2) 0.36016(14) 0.0391(5) Uani 1 1 d . . . . .
C00S C 0.4611(4) 0.6841(3) 0.25519(17) 0.0658(10) Uani 1 1 d . . . . .
H00T H 0.489828 0.701018 0.207588 0.099 Uiso 1 1 calc R U . . .
H00U H 0.382006 0.635437 0.253899 0.099 Uiso 1 1 calc R U . . .
H00V H 0.535969 0.648325 0.279981 0.099 Uiso 1 1 calc R U . . .
C00T C 0.1256(3) 0.3358(3) 0.47357(18) 0.0557(8) Uani 1 1 d . . . . .
H00W H 0.034064 0.362761 0.486737 0.067 Uiso 1 1 calc R U . . .
H00X H 0.115130 0.273920 0.440977 0.067 Uiso 1 1 calc R U . . .
C00U C 0.5722(4) 0.3409(3) 0.72457(18) 0.0666(10) Uani 1 1 d . . . . .
H00Y H 0.633534 0.354200 0.685265 0.100 Uiso 1 1 calc R U . . .
H H 0.625514 0.318347 0.765177 0.100 Uiso 1 1 calc R U . . .
HA H 0.522239 0.407895 0.735501 0.100 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
O001 0.0659(13) 0.0474(12) 0.0517(11) 0.0158(9) -0.0095(10) -0.0044(10)
O002 0.0731(14) 0.0483(12) 0.0429(10) 0.0087(9) 0.0029(10) 0.0047(11)
O003 0.129(3) 0.0367(12) 0.0900(19) 0.0115(12) -0.0001(18) 0.0068(14)
O004 0.101(2) 0.0418(12) 0.0937(19) 0.0098(13) 0.0220(17) -0.0145(14)
C005 0.0400(13) 0.0287(12) 0.0554(16) -0.0029(11) -0.0092(12) 0.0027(10)
C006 0.0452(14) 0.0378(13) 0.0485(15) -0.0054(12) 0.0054(12) 0.0061(12)
C007 0.0366(12) 0.0339(12) 0.0361(12) -0.0045(10) 0.0026(10) -0.0002(10)
C008 0.0373(13) 0.0311(12) 0.0462(13) -0.0024(11) -0.0037(11) 0.0039(10)
C009 0.0394(13) 0.0432(15) 0.0472(14) -0.0062(12) -0.0038(12) -0.0020(12)
C00A 0.062(2) 0.0409(16) 0.0642(19) 0.0131(14) -0.0104(16) -0.0009(14)
C00B 0.0484(16) 0.0470(16) 0.0472(15) -0.0019(12) 0.0102(12) 0.0002(12)
C00C 0.0337(12) 0.0334(12) 0.0400(13) -0.0016(10) -0.0047(10) -0.0025(10)
C00D 0.0451(14) 0.0358(13) 0.0403(13) 0.0014(11) 0.0059(11) 0.0034(11)
C00E 0.0302(11) 0.0321(12) 0.0390(12) -0.0013(10) -0.0039(10) 0.0008(9)
C00F 0.0412(13) 0.0326(12) 0.0396(12) -0.0011(10) 0.0005(11) -0.0044(11)
C00G 0.070(2) 0.0475(16) 0.0516(17) -0.0122(14) -0.0060(16) -0.0003(16)
C00H 0.0450(14) 0.0336(13) 0.0507(15) 0.0036(11) 0.0124(13) 0.0023(11)
C00I 0.0417(13) 0.0321(12) 0.0414(14) -0.0026(10) -0.0039(11) -0.0008(11)
C00J 0.0401(13) 0.0329(12) 0.0512(15) 0.0061(12) -0.0095(12) -0.0005(11)
C00K 0.0448(14) 0.0335(13) 0.0612(17) -0.0022(12) 0.0063(13) -0.0091(11)
C00L 0.0309(11) 0.0282(11) 0.0416(13) 0.0009(10) -0.0046(10) -0.0012(9)
C00M 0.0390(12) 0.0301(12) 0.0422(13) -0.0009(10) 0.0012(11) -0.0028(10)
C00N 0.0646(19) 0.0385(15) 0.0642(19) 0.0097(14) 0.0183(16) 0.0019(14)
C00O 0.0448(14) 0.0371(13) 0.0500(15) -0.0022(12) -0.0152(13) -0.0043(12)
C00P 0.0503(17) 0.0559(18) 0.0637(19) 0.0033(15) -0.0249(15) -0.0046(14)
C00Q 0.0417(13) 0.0378(14) 0.0526(16) -0.0011(11) -0.0034(13) -0.0064(11)
C00R 0.0364(12) 0.0405(13) 0.0405(13) 0.0043(11) -0.0061(10) 0.0011(11)
C00S 0.089(3) 0.064(2) 0.0449(16) 0.0016(15) 0.0069(17) 0.0197(19)
C00T 0.0509(16) 0.0473(16) 0.069(2) 0.0012(15) -0.0167(15) -0.0159(14)
C00U 0.076(2) 0.066(2) 0.0569(19) 0.0157(16) -0.0216(18) -0.0115(19)
_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
O001 C00D 1.369(3) . ?
O001 C00U 1.421(4) . ?
O002 C00R 1.359(3) . ?
O002 C00S 1.426(4) . ?
O003 C00A 1.206(4) . ?
O004 C00N 1.205(4) . ?
C005 H005 0.9300 . ?
C005 C008 1.379(4) . ?
C005 C00J 1.392(4) . ?
C006 H00A 0.9700 . ?
C006 H00B 0.9700 . ?
C006 C007 1.555(4) . ?
C006 C008 1.487(4) . ?
C007 C009 1.533(4) . ?
C007 C00B 1.528(4) . ?
C007 C00E 1.555(3) . ?
C008 C00L 1.404(3) . ?
C009 H00C 0.9600 . ?
C009 H00D 0.9600 . ?
C009 H00E 0.9600 . ?
C00A H00F 0.9300 . ?
C00A C00J 1.469(4) . ?
C00B H00G 0.9600 . ?
C00B H00H 0.9600 . ?
C00B H00I 0.9600 . ?
C00C C00E 1.359(3) . ?
C00C C00M 1.475(3) . ?
C00C C00O 1.554(4) . ?
C00D C00F 1.387(4) . ?
C00D C00H 1.400(4) . ?
C00E C00L 1.479(3) . ?
C00F H00J 0.9300 . ?
C00F C00M 1.393(4) . ?
C00G H00K 0.9600 . ?
C00G H00L 0.9600 . ?
C00G H00M 0.9600 . ?
C00G C00O 1.535(4) . ?
C00H C00K 1.392(4) . ?
C00H C00N 1.469(4) . ?
C00I H00N 0.9300 . ?
C00I C00L 1.392(4) . ?
C00I C00R 1.394(4) . ?
C00J C00R 1.406(4) . ?
C00K H00O 0.9300 . ?
C00K C00Q 1.375(4) . ?
C00M C00Q 1.397(4) . ?
C00N H00P 0.9300 . ?
C00O C00P 1.528(4) . ?
C00O C00T 1.560(4) . ?
C00P H00Q 0.9600 . ?
C00P H00R 0.9600 . ?
C00P H00S 0.9600 . ?
C00Q C00T 1.498(4) . ?
C00S H00T 0.9600 . ?
C00S H00U 0.9600 . ?
C00S H00V 0.9600 . ?
C00T H00W 0.9700 . ?
C00T H00X 0.9700 . ?
C00U H00Y 0.9600 . ?
C00U H 0.9600 . ?
C00U HA 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
C00D O001 C00U 117.4(2) . . ?
C00R O002 C00S 118.2(2) . . ?
C008 C005 H005 119.8 . . ?
C008 C005 C00J 120.4(2) . . ?
C00J C005 H005 119.8 . . ?
H00A C006 H00B 109.0 . . ?
C007 C006 H00A 111.0 . . ?
C007 C006 H00B 111.0 . . ?
C008 C006 H00A 111.0 . . ?
C008 C006 H00B 111.0 . . ?
C008 C006 C007 103.9(2) . . ?
C006 C007 C00E 100.6(2) . . ?
C009 C007 C006 108.2(2) . . ?
C009 C007 C00E 110.2(2) . . ?
C00B C007 C006 108.1(2) . . ?
C00B C007 C009 111.6(2) . . ?
C00B C007 C00E 117.1(2) . . ?
C005 C008 C006 130.3(2) . . ?
C005 C008 C00L 120.0(2) . . ?
C00L C008 C006 109.7(2) . . ?
C007 C009 H00C 109.5 . . ?
C007 C009 H00D 109.5 . . ?
C007 C009 H00E 109.5 . . ?
H00C C009 H00D 109.5 . . ?
H00C C009 H00E 109.5 . . ?
H00D C009 H00E 109.5 . . ?
O003 C00A H00F 118.1 . . ?
O003 C00A C00J 123.8(3) . . ?
C00J C00A H00F 118.1 . . ?
C007 C00B H00G 109.5 . . ?
C007 C00B H00H 109.5 . . ?
C007 C00B H00I 109.5 . . ?
H00G C00B H00H 109.5 . . ?
H00G C00B H00I 109.5 . . ?
H00H C00B H00I 109.5 . . ?
C00E C00C C00M 126.1(2) . . ?
C00E C00C C00O 128.6(2) . . ?
C00M C00C C00O 105.0(2) . . ?
O001 C00D C00F 122.4(2) . . ?
O001 C00D C00H 116.7(2) . . ?
C00F C00D C00H 120.8(2) . . ?
C00C C00E C007 127.7(2) . . ?
C00C C00E C00L 127.1(2) . . ?
C00L C00E C007 105.0(2) . . ?
C00D C00F H00J 120.4 . . ?
C00D C00F C00M 119.1(2) . . ?
C00M C00F H00J 120.4 . . ?
H00K C00G H00L 109.5 . . ?
H00K C00G H00M 109.5 . . ?
H00L C00G H00M 109.5 . . ?
C00O C00G H00K 109.5 . . ?
C00O C00G H00L 109.5 . . ?
C00O C00G H00M 109.5 . . ?
C00D C00H C00N 120.9(3) . . ?
C00K C00H C00D 119.0(2) . . ?
C00K C00H C00N 120.1(3) . . ?
C00L C00I H00N 120.4 . . ?
C00L C00I C00R 119.3(2) . . ?
C00R C00I H00N 120.4 . . ?
C005 C00J C00A 119.5(3) . . ?
C005 C00J C00R 119.6(2) . . ?
C00R C00J C00A 120.8(3) . . ?
C00H C00K H00O 119.7 . . ?
C00Q C00K C00H 120.6(3) . . ?
C00Q C00K H00O 119.7 . . ?
C008 C00L C00E 109.3(2) . . ?
C00I C00L C008 120.3(2) . . ?
C00I C00L C00E 129.9(2) . . ?
C00F C00M C00C 129.0(2) . . ?
C00F C00M C00Q 120.1(2) . . ?
C00Q C00M C00C 110.5(2) . . ?
O004 C00N C00H 124.9(3) . . ?
O004 C00N H00P 117.6 . . ?
C00H C00N H00P 117.6 . . ?
C00C C00O C00T 101.0(2) . . ?
C00G C00O C00C 111.2(2) . . ?
C00G C00O C00T 107.9(2) . . ?
C00P C00O C00C 116.3(2) . . ?
C00P C00O C00G 111.1(3) . . ?
C00P C00O C00T 108.6(2) . . ?
C00O C00P H00Q 109.5 . . ?
C00O C00P H00R 109.5 . . ?
C00O C00P H00S 109.5 . . ?
H00Q C00P H00R 109.5 . . ?
H00Q C00P H00S 109.5 . . ?
H00R C00P H00S 109.5 . . ?
C00K C00Q C00M 120.0(3) . . ?
C00K C00Q C00T 130.9(3) . . ?
C00M C00Q C00T 109.0(2) . . ?
O002 C00R C00I 123.8(2) . . ?
O002 C00R C00J 115.9(2) . . ?
C00I C00R C00J 120.3(2) . . ?
O002 C00S H00T 109.5 . . ?
O002 C00S H00U 109.5 . . ?
O002 C00S H00V 109.5 . . ?
H00T C00S H00U 109.5 . . ?
H00T C00S H00V 109.5 . . ?
H00U C00S H00V 109.5 . . ?
C00O C00T H00W 110.8 . . ?
C00O C00T H00X 110.8 . . ?
C00Q C00T C00O 104.5(2) . . ?
C00Q C00T H00W 110.8 . . ?
C00Q C00T H00X 110.8 . . ?
H00W C00T H00X 108.9 . . ?
O001 C00U H00Y 109.5 . . ?
O001 C00U H 109.5 . . ?
O001 C00U HA 109.5 . . ?
H00Y C00U H 109.5 . . ?
H00Y C00U HA 109.5 . . ?
H C00U HA 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
O001 C00D C00F C00M -179.8(2) . . . . ?
O001 C00D C00H C00K -176.3(2) . . . . ?
O001 C00D C00H C00N 4.3(4) . . . . ?
O003 C00A C00J C005 -2.3(5) . . . . ?
O003 C00A C00J C00R 178.4(3) . . . . ?
C005 C008 C00L C00E 176.2(2) . . . . ?
C005 C008 C00L C00I 3.1(4) . . . . ?
C005 C00J C00R O002 -178.8(2) . . . . ?
C005 C00J C00R C00I 0.3(4) . . . . ?
C006 C007 C00E C00C -144.1(3) . . . . ?
C006 C007 C00E C00L 31.2(2) . . . . ?
C006 C008 C00L C00E -2.6(3) . . . . ?
C006 C008 C00L C00I -175.8(2) . . . . ?
C007 C006 C008 C005 -155.8(3) . . . . ?
C007 C006 C008 C00L 22.9(3) . . . . ?
C007 C00E C00L C008 -18.9(3) . . . . ?
C007 C00E C00L C00I 153.4(3) . . . . ?
C008 C005 C00J C00A 179.8(2) . . . . ?
C008 C005 C00J C00R -1.0(4) . . . . ?
C008 C006 C007 C009 83.3(3) . . . . ?
C008 C006 C007 C00B -155.7(2) . . . . ?
C008 C006 C007 C00E -32.4(3) . . . . ?
C009 C007 C00E C00C 101.8(3) . . . . ?
C009 C007 C00E C00L -82.9(2) . . . . ?
C00A C00J C00R O002 0.5(4) . . . . ?
C00A C00J C00R C00I 179.6(3) . . . . ?
C00B C007 C00E C00C -27.3(4) . . . . ?
C00B C007 C00E C00L 148.0(2) . . . . ?
C00C C00E C00L C008 156.5(3) . . . . ?
C00C C00E C00L C00I -31.2(4) . . . . ?
C00C C00M C00Q C00K 178.8(3) . . . . ?
C00C C00M C00Q C00T -1.0(3) . . . . ?
C00C C00O C00T C00Q -29.8(3) . . . . ?
C00D C00F C00M C00C -178.2(3) . . . . ?
C00D C00F C00M C00Q -5.4(4) . . . . ?
C00D C00H C00K C00Q -2.8(4) . . . . ?
C00D C00H C00N O004 -175.6(3) . . . . ?
C00E C00C C00M C00F -31.8(4) . . . . ?
C00E C00C C00M C00Q 154.9(3) . . . . ?
C00E C00C C00O C00G 101.7(3) . . . . ?
C00E C00C C00O C00P -26.8(4) . . . . ?
C00E C00C C00O C00T -144.0(3) . . . . ?
C00F C00D C00H C00K 2.2(4) . . . . ?
C00F C00D C00H C00N -177.2(3) . . . . ?
C00F C00M C00Q C00K 4.8(4) . . . . ?
C00F C00M C00Q C00T -175.1(3) . . . . ?
C00G C00O C00T C00Q 86.9(3) . . . . ?
C00H C00D C00F C00M 1.9(4) . . . . ?
C00H C00K C00Q C00M -0.7(4) . . . . ?
C00H C00K C00Q C00T 179.2(3) . . . . ?
C00J C005 C008 C006 177.9(3) . . . . ?
C00J C005 C008 C00L -0.7(4) . . . . ?
C00K C00H C00N O004 5.0(5) . . . . ?
C00K C00Q C00T C00O -159.6(3) . . . . ?
C00L C00I C00R O002 -179.0(2) . . . . ?
C00L C00I C00R C00J 2.0(4) . . . . ?
C00M C00C C00E C007 -17.4(4) . . . . ?
C00M C00C C00E C00L 168.3(2) . . . . ?
C00M C00C C00O C00G -85.0(3) . . . . ?
C00M C00C C00O C00P 146.6(3) . . . . ?
C00M C00C C00O C00T 29.3(3) . . . . ?
C00M C00Q C00T C00O 20.2(3) . . . . ?
C00N C00H C00K C00Q 176.6(3) . . . . ?
C00O C00C C00E C007 154.6(3) . . . . ?
C00O C00C C00E C00L -19.7(4) . . . . ?
C00O C00C C00M C00F 154.7(3) . . . . ?
C00O C00C C00M C00Q -18.7(3) . . . . ?
C00P C00O C00T C00Q -152.6(3) . . . . ?
C00R C00I C00L C008 -3.7(4) . . . . ?
C00R C00I C00L C00E -175.2(2) . . . . ?
C00S O002 C00R C00I -3.0(4) . . . . ?
C00S O002 C00R C00J 176.1(3) . . . . ?
C00U O001 C00D C00F 3.3(4) . . . . ?
C00U O001 C00D C00H -178.3(3) . . . . ?
_shelx_res_file
;
TITL mo_CNS_Jin_12_0m_a.res in P2(1)2(1)2(1)
mo_cns_jin_12_0m_a.res
created by SHELXL-2018/3 at 16:38:16 on 18-Dec-2023
REM Old TITL mo_CNS_Jin_12_0m in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.150, Rweak 0.030, Alpha 0.005, Orientation as input
REM Flack x = 0.413 ( 0.732 ) from Parsons' quotients
REM Formula found by SHELXT: C26 O4
CELL 0.71073 9.6167 12.0209 18.8367 90 90 90
ZERR 4 0.0008 0.001 0.0016 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H O
UNIT 104 112 16
L.S. 10
PLAN 2
SIZE 0.117 0.137 0.175
TEMP 19.85
CONF
BOND $H
LIST 4
MORE -1
fmap 2
acta
OMIT 0 2 0
OMIT -1 1 2
OMIT 1 1 2
OMIT -1 1 1
OMIT 1 1 1
OMIT 2 0 3
OMIT 0 2 3
OMIT 0 1 2
REM
REM
REM
WGHT 0.044600 0.520500
FVAR 0.66328
O001 3 0.476398 0.255456 0.706449 11.00000 0.06586 0.04744 =
0.05170 0.01580 -0.00949 -0.00440
O002 3 0.424688 0.784537 0.291006 11.00000 0.07309 0.04826 =
0.04289 0.00867 0.00294 0.00471
O003 3 0.349735 1.075437 0.381643 11.00000 0.12869 0.03672 =
0.08996 0.01148 -0.00008 0.00681
O004 3 0.206807 0.012962 0.667112 11.00000 0.10052 0.04179 =
0.09373 0.00982 0.02201 -0.01453
C005 1 0.320775 0.881007 0.465437 11.00000 0.04000 0.02874 =
0.05536 -0.00290 -0.00922 0.00274
AFIX 43
H005 2 0.304777 0.948393 0.488275 11.00000 -1.20000
AFIX 0
C006 1 0.271331 0.762380 0.578156 11.00000 0.04522 0.03783 =
0.04854 -0.00539 0.00539 0.00606
AFIX 23
H00A 2 0.171449 0.762493 0.585333 11.00000 -1.20000
H00B 2 0.312920 0.818488 0.608468 11.00000 -1.20000
AFIX 0
C007 1 0.333866 0.645558 0.593635 11.00000 0.03662 0.03393 =
0.03612 -0.00453 0.00260 -0.00018
C008 1 0.306386 0.782611 0.502345 11.00000 0.03731 0.03112 =
0.04624 -0.00236 -0.00373 0.00386
C009 1 0.488528 0.660017 0.611058 11.00000 0.03936 0.04318 =
0.04715 -0.00616 -0.00380 -0.00195
AFIX 137
H00C 2 0.531634 0.705376 0.575349 11.00000 -1.50000
H00D 2 0.532782 0.588455 0.612208 11.00000 -1.50000
H00E 2 0.498022 0.695276 0.656529 11.00000 -1.50000
AFIX 0
C00A 1 0.373410 0.985690 0.355732 11.00000 0.06167 0.04091 =
0.06420 0.01309 -0.01036 -0.00090
AFIX 43
H00F 2 0.402413 0.983243 0.308659 11.00000 -1.20000
AFIX 0
C00B 1 0.254035 0.594829 0.655822 11.00000 0.04841 0.04697 =
0.04721 -0.00192 0.01020 0.00019
AFIX 137
H00G 2 0.237391 0.650971 0.691057 11.00000 -1.50000
H00H 2 0.307738 0.535629 0.676276 11.00000 -1.50000
H00I 2 0.166806 0.566006 0.639213 11.00000 -1.50000
AFIX 0
C00C 1 0.285174 0.480932 0.506160 11.00000 0.03365 0.03336 =
0.03997 -0.00160 -0.00473 -0.00253
C00D 1 0.387067 0.275675 0.651388 11.00000 0.04506 0.03583 =
0.04035 0.00141 0.00594 0.00338
C00E 1 0.316315 0.589081 0.519903 11.00000 0.03021 0.03213 =
0.03902 -0.00133 -0.00387 0.00081
C00F 1 0.392275 0.372631 0.611594 11.00000 0.04116 0.03261 =
0.03964 -0.00105 0.00051 -0.00439
AFIX 43
H00J 2 0.458186 0.427044 0.621568 11.00000 -1.20000
AFIX 0
C00G 1 0.321080 0.376484 0.389865 11.00000 0.07007 0.04747 =
0.05155 -0.01217 -0.00598 -0.00033
AFIX 137
H00K 2 0.386156 0.431735 0.374041 11.00000 -1.50000
H00L 2 0.274282 0.344962 0.349592 11.00000 -1.50000
H00M 2 0.369799 0.318926 0.414954 11.00000 -1.50000
AFIX 0
C00H 1 0.290883 0.191886 0.635445 11.00000 0.04501 0.03362 =
0.05068 0.00363 0.01243 0.00225
C00I 1 0.372210 0.678287 0.397367 11.00000 0.04165 0.03215 =
0.04142 -0.00264 -0.00394 -0.00076
AFIX 43
H00N 2 0.392225 0.610941 0.375321 11.00000 -1.20000
AFIX 0
C00J 1 0.359116 0.880019 0.394178 11.00000 0.04005 0.03291 =
0.05116 0.00613 -0.00946 -0.00046
C00K 1 0.203117 0.205446 0.577323 11.00000 0.04479 0.03351 =
0.06117 -0.00221 0.00626 -0.00906
AFIX 43
H00O 2 0.141655 0.148906 0.565032 11.00000 -1.20000
AFIX 0
C00L 1 0.328916 0.680631 0.467854 11.00000 0.03089 0.02824 =
0.04161 0.00088 -0.00463 -0.00122
C00M 1 0.297507 0.387456 0.556493 11.00000 0.03898 0.03014 =
0.04221 -0.00090 0.00121 -0.00277
C00N 1 0.281040 0.091377 0.679516 11.00000 0.06461 0.03854 =
0.06419 0.00970 0.01831 0.00190
AFIX 43
H00P 2 0.336203 0.087998 0.720011 11.00000 -1.20000
AFIX 0
C00O 1 0.213939 0.430584 0.439450 11.00000 0.04481 0.03711 =
0.04998 -0.00220 -0.01516 -0.00432
C00P 1 0.116603 0.507715 0.398338 11.00000 0.05033 0.05591 =
0.06368 0.00326 -0.02487 -0.00463
AFIX 137
H00Q 2 0.058222 0.547281 0.431071 11.00000 -1.50000
H00R 2 0.059830 0.464454 0.366793 11.00000 -1.50000
H00S 2 0.170613 0.559860 0.371326 11.00000 -1.50000
AFIX 0
C00Q 1 0.206489 0.301693 0.537920 11.00000 0.04168 0.03782 =
0.05255 -0.00111 -0.00337 -0.00641
C00R 1 0.385246 0.778038 0.360164 11.00000 0.03638 0.04047 =
0.04052 0.00435 -0.00610 0.00113
C00S 1 0.461100 0.684120 0.255190 11.00000 0.08882 0.06370 =
0.04494 0.00159 0.00693 0.01972
AFIX 137
H00T 2 0.489828 0.701018 0.207588 11.00000 -1.50000
H00U 2 0.382006 0.635437 0.253899 11.00000 -1.50000
H00V 2 0.535969 0.648325 0.279981 11.00000 -1.50000
AFIX 0
C00T 1 0.125582 0.335828 0.473572 11.00000 0.05085 0.04734 =
0.06905 0.00116 -0.01671 -0.01585
AFIX 23
H00W 2 0.034064 0.362761 0.486737 11.00000 -1.20000
H00X 2 0.115130 0.273920 0.440977 11.00000 -1.20000
AFIX 0
C00U 1 0.572196 0.340909 0.724569 11.00000 0.07646 0.06627 =
0.05692 0.01573 -0.02156 -0.01146
AFIX 137
H00Y 2 0.633534 0.354200 0.685265 11.00000 -1.50000
H 2 0.625514 0.318347 0.765177 11.00000 -1.50000
HA 2 0.522239 0.407895 0.735501 11.00000 -1.50000
AFIX 0
HKLF 4
REM mo_CNS_Jin_12_0m_a.res in P2(1)2(1)2(1)
REM wR2 = 0.1297, GooF = S = 1.025, Restrained GooF = 1.025 for all data
REM R1 = 0.0545 for 4704 Fo > 4sig(Fo) and 0.0766 for all 6111 data
REM 277 parameters refined using 0 restraints
END
WGHT 0.0448 0.5186
REM Highest difference peak 0.159, deepest hole -0.192, 1-sigma level 0.040
Q1 1 0.0620 0.6721 0.5637 11.00000 0.05 0.16
Q2 1 0.3554 0.7376 0.4816 11.00000 0.05 0.16
;
_shelx_res_checksum 8618
_olex2_submission_special_instructions 'No special instructions were received'