# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_cda_0ma
_database_code_depnum_ccdc_archive 'CCDC 2203890'
loop_
_audit_author_name
_audit_author_address
Fruzinski
;Technical University of Lodz
Poland
;
_audit_update_record             
;
2022-08-28 deposited with the CCDC.	2022-11-04 downloaded from the CCDC.
;
_audit_creation_date             2022-04-22
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            Fmoc-b-cyclopropyl-(S)-Ala-OH
_chemical_name_systematic        
;
(2S)-2-[cyclopropyl(9H-fluoren-9-ylmethoxycarbonyl)amino]propanoic acid  
;
_chemical_formula_moiety         'C13 H21 N O5'
_chemical_formula_sum            'C13 H21 N O5'
_chemical_formula_weight         271.31
_chemical_absolute_configuration rm
_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           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
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                   9.589(2)
_cell_length_b                   12.661(3)
_cell_length_c                   11.779(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1430.0(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    65854
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.758
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1381
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            63207
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         50.758
_diffrn_reflns_theta_min         2.362
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                13453
_reflns_number_total             15085
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         15085
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0533
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0904P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1381
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1.0(4)
 -0.0(4)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N N 0.82814(5) 0.31903(4) 0.02125(5) 0.01286(7) Uani 1 1 d . . . . .
C1 C 0.73241(6) 0.25352(4) -0.02449(6) 0.01346(7) Uani 1 1 d . . . . .
C2 C 0.78737(7) 0.15532(5) -0.08128(7) 0.01694(9) Uani 1 1 d . . . . .
O1 O 0.60637(5) 0.27398(4) -0.01998(6) 0.01887(9) Uani 1 1 d . . . . .
C3 C 0.78472(6) 0.41398(4) 0.08061(5) 0.01301(7) Uani 1 1 d . . . . .
C4 C 0.72203(7) 0.38885(6) 0.19845(6) 0.01751(9) Uani 1 1 d . . . . .
C5 C 0.82090(9) 0.32802(6) 0.27356(6) 0.02079(11) Uani 1 1 d . . . . .
C6 C 0.79739(14) 0.32920(9) 0.40015(8) 0.02869(16) Uani 1 1 d . . . . .
C7 C 0.92247(12) 0.38454(10) 0.35017(8) 0.02852(17) Uani 1 1 d . . . . .
C8 C 0.67770(6) 0.47714(5) 0.00982(6) 0.01460(8) Uani 1 1 d . . . . .
O2 O 0.57507(6) 0.51847(5) 0.04870(6) 0.02139(10) Uani 1 1 d . . . . .
O3 O 0.71791(5) 0.48366(4) -0.09861(5) 0.01580(7) Uani 1 1 d . . . . .
C9 C 0.61823(7) 0.53343(6) -0.17465(7) 0.01836(10) Uani 1 1 d . . . . .
C10 C 0.68725(9) 0.54419(7) -0.28854(7) 0.02134(11) Uani 1 1 d . . . . .
C11 C 0.91506(6) 0.48312(5) 0.09579(5) 0.01410(8) Uani 1 1 d . . . . .
O4 O 1.03081(6) 0.45449(5) 0.07118(6) 0.02036(9) Uani 1 1 d . . . . .
O5 O 0.88218(6) 0.57672(4) 0.14054(6) 0.01906(9) Uani 1 1 d . . . . .
C12 C 0.99869(10) 0.64706(6) 0.16601(8) 0.02228(12) Uani 1 1 d . . . . .
C13 C 0.94606(14) 0.75885(7) 0.16291(11) 0.02974(17) Uani 1 1 d . . . . .
H4A H 0.646(3) 0.349(2) 0.189(2) 0.035(6) Uiso 1 1 d . . . . .
H4B H 0.699(2) 0.457(2) 0.235(2) 0.026(5) Uiso 1 1 d . . . . .
H5 H 0.846(3) 0.254(2) 0.239(2) 0.030(5) Uiso 1 1 d . . . . .
H6A H 0.721(3) 0.379(3) 0.431(3) 0.038(6) Uiso 1 1 d . . . . .
H7A H 0.924(2) 0.466(2) 0.349(3) 0.034(6) Uiso 1 1 d . . . . .
H7B H 1.018(3) 0.348(2) 0.359(2) 0.032(5) Uiso 1 1 d . . . . .
H2A H 0.887(3) 0.152(2) -0.075(3) 0.038(6) Uiso 1 1 d . . . . .
H12A H 1.078(2) 0.635(2) 0.114(2) 0.030(5) Uiso 1 1 d . . . . .
H12B H 1.027(3) 0.632(3) 0.238(3) 0.043(6) Uiso 1 1 d . . . . .
H13A H 1.015(2) 0.801(2) 0.175(2) 0.029(5) Uiso 1 1 d . . . . .
H13B H 0.875(4) 0.775(4) 0.210(4) 0.061(10) Uiso 1 1 d . . . . .
H9A H 0.533(3) 0.494(3) -0.175(3) 0.041(7) Uiso 1 1 d . . . . .
H9B H 0.592(2) 0.604(2) -0.144(2) 0.028(5) Uiso 1 1 d . . . . .
H10A H 0.625(2) 0.5793(19) -0.340(2) 0.025(4) Uiso 1 1 d . . . . .
H10B H 0.709(3) 0.469(3) -0.321(3) 0.044(7) Uiso 1 1 d . . . . .
H10C H 0.772(2) 0.5853(19) -0.292(2) 0.024(4) Uiso 1 1 d . . . . .
H13C H 0.904(4) 0.771(3) 0.096(4) 0.059(9) Uiso 1 1 d . . . . .
H2B H 0.726(3) 0.099(3) -0.048(4) 0.055(8) Uiso 1 1 d . . . . .
H2C H 0.757(6) 0.162(5) -0.167(5) 0.091(15) Uiso 1 1 d . . . . .
H6B H 0.813(2) 0.264(2) 0.442(3) 0.038(6) Uiso 1 1 d . . . . .
H H 0.9159(18) 0.3055(17) 0.0137(18) 0.017(3) Uiso 1 1 d . . . . .


_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
N C1 1.3494(8) . ?
N C3 1.4517(8) . ?
N H 0.863(17) . ?
C1 C2 1.5069(9) . ?
C1 O1 1.2371(8) . ?
C2 H2A 0.96(3) . ?
C2 H2B 1.00(4) . ?
C2 H2C 1.05(6) . ?
C3 C4 1.5457(9) . ?
C3 C8 1.5453(9) . ?
C3 C11 1.5364(9) . ?
C4 C5 1.5082(11) . ?
C4 H4A 0.89(3) . ?
C4 H4B 0.99(3) . ?
C5 C6 1.5081(12) . ?
C5 C7 1.5083(14) . ?
C5 H5 1.05(3) . ?
C6 C7 1.5086(16) . ?
C6 H6A 1.03(3) . ?
C6 H6B 0.97(3) . ?
C7 H7A 1.04(3) . ?
C7 H7B 1.03(3) . ?
C8 O2 1.2050(8) . ?
C8 O3 1.3366(9) . ?
O3 C9 1.4536(9) . ?
C9 C10 1.5021(12) . ?
C9 H9A 0.96(3) . ?
C9 H9B 0.99(3) . ?
C10 H10A 0.96(2) . ?
C10 H10B 1.05(3) . ?
C10 H10C 0.96(2) . ?
C11 O4 1.2031(8) . ?
C11 O5 1.3347(8) . ?
O5 C12 1.4600(10) . ?
C12 C13 1.5031(13) . ?
C12 H12A 0.99(2) . ?
C12 H12B 0.91(4) . ?
C13 H13A 0.87(2) . ?
C13 H13B 0.90(4) . ?
C13 H13C 0.90(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
C1 N C3 120.41(5) . . ?
C1 N H 120.0(14) . . ?
C3 N H 119.6(14) . . ?
N C1 C2 116.51(5) . . ?
O1 C1 N 121.25(6) . . ?
O1 C1 C2 122.24(6) . . ?
C1 C2 H2A 110.1(19) . . ?
C1 C2 H2B 102(2) . . ?
C1 C2 H2C 105(3) . . ?
H2A C2 H2B 122(3) . . ?
H2A C2 H2C 111(4) . . ?
H2B C2 H2C 106(4) . . ?
N C3 C4 111.93(5) . . ?
N C3 C8 111.05(5) . . ?
N C3 C11 107.13(5) . . ?
C8 C3 C4 109.44(5) . . ?
C11 C3 C4 109.22(5) . . ?
C11 C3 C8 107.95(5) . . ?
C3 C4 H4A 108.9(19) . . ?
C3 C4 H4B 107.3(15) . . ?
C5 C4 C3 112.80(6) . . ?
C5 C4 H4A 107.0(19) . . ?
C5 C4 H4B 109.4(15) . . ?
H4A C4 H4B 112(2) . . ?
C4 C5 C7 120.97(8) . . ?
C4 C5 H5 112.1(15) . . ?
C6 C5 C4 118.75(8) . . ?
C6 C5 C7 60.02(7) . . ?
C6 C5 H5 115.1(16) . . ?
C7 C5 H5 120.3(14) . . ?
C5 C6 C7 60.00(6) . . ?
C5 C6 H6A 117.2(18) . . ?
C5 C6 H6B 118(2) . . ?
C7 C6 H6A 114.3(17) . . ?
C7 C6 H6B 117.9(15) . . ?
H6A C6 H6B 117(3) . . ?
C5 C7 C6 59.98(7) . . ?
C5 C7 H7A 118.5(15) . . ?
C5 C7 H7B 114.9(16) . . ?
C6 C7 H7A 118.9(14) . . ?
C6 C7 H7B 117.3(16) . . ?
H7A C7 H7B 116(2) . . ?
O2 C8 C3 124.19(7) . . ?
O2 C8 O3 124.89(6) . . ?
O3 C8 C3 110.85(5) . . ?
C8 O3 C9 115.20(5) . . ?
O3 C9 C10 107.45(6) . . ?
O3 C9 H9A 110(2) . . ?
O3 C9 H9B 109.5(14) . . ?
C10 C9 H9A 115(2) . . ?
C10 C9 H9B 110.7(15) . . ?
H9A C9 H9B 105(2) . . ?
C9 C10 H10A 109.3(14) . . ?
C9 C10 H10B 109.5(19) . . ?
C9 C10 H10C 117.3(14) . . ?
H10A C10 H10B 108(2) . . ?
H10A C10 H10C 104.2(19) . . ?
H10B C10 H10C 108(2) . . ?
O4 C11 C3 123.42(6) . . ?
O4 C11 O5 125.50(6) . . ?
O5 C11 C3 111.08(5) . . ?
C11 O5 C12 116.23(6) . . ?
O5 C12 C13 108.21(8) . . ?
O5 C12 H12A 111.3(15) . . ?
O5 C12 H12B 107(2) . . ?
C13 C12 H12A 112.9(16) . . ?
C13 C12 H12B 108(2) . . ?
H12A C12 H12B 109(2) . . ?
C12 C13 H13A 108.7(17) . . ?
C12 C13 H13B 117(3) . . ?
C12 C13 H13C 109(3) . . ?
H13A C13 H13B 110(3) . . ?
H13A C13 H13C 113(3) . . ?
H13B C13 H13C 99(4) . . ?

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
N C3 C4 C5 57.03(7) . . . . ?
N C3 C8 O2 138.15(7) . . . . ?
N C3 C8 O3 -44.73(7) . . . . ?
N C3 C11 O4 -6.53(9) . . . . ?
N C3 C11 O5 174.27(6) . . . . ?
C1 N C3 C4 73.92(7) . . . . ?
C1 N C3 C8 -48.73(7) . . . . ?
C1 N C3 C11 -166.38(6) . . . . ?
C3 N C1 C2 -178.19(6) . . . . ?
C3 N C1 O1 2.10(10) . . . . ?
C3 C4 C5 C6 159.61(8) . . . . ?
C3 C4 C5 C7 89.21(9) . . . . ?
C3 C8 O3 C9 174.71(5) . . . . ?
C3 C11 O5 C12 176.13(6) . . . . ?
C4 C3 C8 O2 14.08(9) . . . . ?
C4 C3 C8 O3 -168.80(5) . . . . ?
C4 C3 C11 O4 114.90(8) . . . . ?
C4 C3 C11 O5 -64.30(7) . . . . ?
C4 C5 C6 C7 -111.17(10) . . . . ?
C4 C5 C7 C6 107.54(9) . . . . ?
C8 C3 C4 C5 -179.42(6) . . . . ?
C8 C3 C11 O4 -126.19(7) . . . . ?
C8 C3 C11 O5 54.61(7) . . . . ?
C8 O3 C9 C10 173.95(6) . . . . ?
O2 C8 O3 C9 -8.19(10) . . . . ?
C11 C3 C4 C5 -61.44(7) . . . . ?
C11 C3 C8 O2 -104.69(7) . . . . ?
C11 C3 C8 O3 72.43(6) . . . . ?
C11 O5 C12 C13 154.27(8) . . . . ?
O4 C11 O5 C12 -3.05(12) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.0(4)
2 -0.0(4)

####################################################################### 
# 
# 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_kk1
_database_code_depnum_ccdc_archive 'CCDC 2203892'
loop_
_audit_author_name
_audit_author_address
Fruzinski
;Technical University of Lodz
Poland
;
_audit_update_record             
;
2022-08-28 deposited with the CCDC.	2022-11-04 downloaded from the CCDC.
;
_audit_creation_date             2022-04-22
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'2-(cyclopropylmethyl)-2-acetamidopropanedioic acid'
_chemical_formula_moiety         'C9 H13 N O5'
_chemical_formula_sum            'C9 H13 N O5'
_chemical_formula_weight         215.20
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.49868(19)
_cell_length_b                   8.0934(2)
_cell_length_c                   9.4854(2)
_cell_angle_alpha                83.844(2)
_cell_angle_beta                 73.807(2)
_cell_angle_gamma                69.194(3)
_cell_volume                     516.76(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      78.723
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15293
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.723
_diffrn_reflns_theta_min         4.855
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2043
_reflns_number_total             2079
_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 > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.0115(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2079
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0282
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0314P)²+0.2314P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0719
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5A)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 N(H)
2.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O4 O 0.57783(10) 0.78324(9) 0.50868(7) 0.01449(18) Uani 1 1 d . . . . .
O3 O 1.02664(10) 0.67385(10) 0.33245(8) 0.01475(18) Uani 1 1 d . . . . .
H3 H 1.136619 0.682015 0.299688 0.022 Uiso 1 1 calc R U . . .
O5 O 0.59884(11) 0.94986(9) 0.30353(8) 0.01487(18) Uani 1 1 d . . . . .
H5 H 0.540885 1.031798 0.361625 0.022 Uiso 1 1 calc R U . . .
O1 O 0.36835(10) 0.71403(10) 0.25905(8) 0.01600(18) Uani 1 1 d . . . . .
O2 O 1.06486(11) 0.60678(10) 0.10022(8) 0.01827(19) Uani 1 1 d . . . . .
N N 0.68749(12) 0.65956(11) 0.14145(9) 0.01169(19) Uani 1 1 d . . . . .
H H 0.774513 0.646411 0.058405 0.014 Uiso 1 1 calc R U . . .
C1 C 0.49848(15) 0.69811(13) 0.14170(11) 0.0127(2) Uani 1 1 d . . . . .
C3 C 0.75270(14) 0.63884(13) 0.27526(10) 0.0113(2) Uani 1 1 d . . . . .
C9 C 0.62963(14) 0.79880(13) 0.37618(11) 0.0115(2) Uani 1 1 d . . . . .
C8 C 0.96693(14) 0.63876(12) 0.22529(11) 0.0115(2) Uani 1 1 d . . . . .
C4 C 0.74832(15) 0.46481(13) 0.35742(11) 0.0132(2) Uani 1 1 d . . . . .
H4A H 0.785549 0.461210 0.448073 0.016 Uiso 1 1 calc R U . . .
H4B H 0.614277 0.463390 0.383019 0.016 Uiso 1 1 calc R U . . .
C5 C 0.88366(15) 0.30200(13) 0.27005(11) 0.0148(2) Uani 1 1 d . . . . .
H5A H 0.868728 0.297261 0.171310 0.018 Uiso 1 1 calc R U . . .
C2 C 0.45435(16) 0.72867(15) -0.00600(11) 0.0182(2) Uani 1 1 d . . . . .
H2A H 0.350935 0.684355 -0.004724 0.027 Uiso 1 1 calc R U . . .
H2B H 0.570990 0.668150 -0.079697 0.027 Uiso 1 1 calc R U . . .
H2C H 0.412954 0.853018 -0.027918 0.027 Uiso 1 1 calc R U . . .
C6 C 1.08907(16) 0.21057(14) 0.29028(13) 0.0210(2) Uani 1 1 d . . . . .
H6A H 1.193631 0.155307 0.205245 0.025 Uiso 1 1 calc R U . . .
H6B H 1.129504 0.261847 0.358607 0.025 Uiso 1 1 calc R U . . .
C7 C 0.93124(17) 0.12960(14) 0.35212(13) 0.0210(2) Uani 1 1 d . . . . .
H7A H 0.941119 0.025326 0.304455 0.025 Uiso 1 1 calc R U . . .
H7B H 0.877024 0.131813 0.457741 0.025 Uiso 1 1 calc R U . . .


_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
O4 C9 1.2145(12) . ?
O3 H3 0.8200 . ?
O3 C8 1.3117(12) . ?
O5 H5 0.8200 . ?
O5 C9 1.3154(12) . ?
O1 C1 1.2423(13) . ?
O2 C8 1.2077(12) . ?
N H 0.8600 . ?
N C1 1.3380(13) . ?
N C3 1.4561(12) . ?
C1 C2 1.5032(14) . ?
C3 C9 1.5390(13) . ?
C3 C8 1.5427(13) . ?
C3 C4 1.5412(13) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.5061(14) . ?
C5 H5A 0.9800 . ?
C5 C6 1.5105(14) . ?
C5 C7 1.4995(15) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.5018(16) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 O3 H3 109.5 . . ?
C9 O5 H5 109.5 . . ?
C1 N H 118.5 . . ?
C1 N C3 123.05(8) . . ?
C3 N H 118.5 . . ?
O1 C1 N 120.74(9) . . ?
O1 C1 C2 122.99(9) . . ?
N C1 C2 116.21(9) . . ?
N C3 C9 110.62(8) . . ?
N C3 C8 105.51(8) . . ?
N C3 C4 112.41(8) . . ?
C9 C3 C8 107.48(7) . . ?
C9 C3 C4 110.90(8) . . ?
C4 C3 C8 109.66(8) . . ?
O4 C9 O5 125.20(9) . . ?
O4 C9 C3 122.19(9) . . ?
O5 C9 C3 112.50(8) . . ?
O3 C8 C3 112.70(8) . . ?
O2 C8 O3 125.59(9) . . ?
O2 C8 C3 121.70(9) . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C5 C4 C3 113.55(8) . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C4 C5 H5A 116.1 . . ?
C4 C5 C6 119.74(9) . . ?
C6 C5 H5A 116.1 . . ?
C7 C5 C4 117.35(9) . . ?
C7 C5 H5A 116.1 . . ?
C7 C5 C6 59.86(7) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C5 C6 H6A 117.8 . . ?
C5 C6 H6B 117.8 . . ?
H6A C6 H6B 114.9 . . ?
C7 C6 C5 59.71(7) . . ?
C7 C6 H6A 117.8 . . ?
C7 C6 H6B 117.8 . . ?
C5 C7 C6 60.43(7) . . ?
C5 C7 H7A 117.7 . . ?
C5 C7 H7B 117.7 . . ?
C6 C7 H7A 117.7 . . ?
C6 C7 H7B 117.7 . . ?
H7A C7 H7B 114.8 . . ?

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
N C3 C9 O4 141.10(9) . . . . ?
N C3 C9 O5 -42.47(11) . . . . ?
N C3 C8 O3 160.91(8) . . . . ?
N C3 C8 O2 -20.01(12) . . . . ?
N C3 C4 C5 61.87(11) . . . . ?
C1 N C3 C9 -51.34(12) . . . . ?
C1 N C3 C8 -167.29(9) . . . . ?
C1 N C3 C4 73.24(11) . . . . ?
C3 N C1 O1 -1.78(15) . . . . ?
C3 N C1 C2 175.45(9) . . . . ?
C3 C4 C5 C6 94.95(11) . . . . ?
C3 C4 C5 C7 164.12(9) . . . . ?
C9 C3 C8 O3 42.83(11) . . . . ?
C9 C3 C8 O2 -138.08(10) . . . . ?
C9 C3 C4 C5 -173.71(8) . . . . ?
C8 C3 C9 O4 -104.19(10) . . . . ?
C8 C3 C9 O5 72.23(10) . . . . ?
C8 C3 C4 C5 -55.16(11) . . . . ?
C4 C3 C9 O4 15.66(13) . . . . ?
C4 C3 C9 O5 -167.91(8) . . . . ?
C4 C3 C8 O3 -77.82(10) . . . . ?
C4 C3 C8 O2 101.27(11) . . . . ?
C4 C5 C6 C7 106.26(11) . . . . ?
C4 C5 C7 C6 -110.22(10) . . . . ?

_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_kk_white
_database_code_depnum_ccdc_archive 'CCDC 2203894'
loop_
_audit_author_name
_audit_author_address
Fruzinski
;Technical University of Lodz
Poland
;
_audit_update_record             
;
2022-08-28 deposited with the CCDC.	2022-11-04 downloaded from the CCDC.
;
_audit_creation_date             2022-05-16
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'diethyl 2-acetamido-2-(cyclopropylmethyl)malonate'
_chemical_formula_moiety         'C21 H21 N O4'
_chemical_formula_sum            'C21 H21 N O4'
_chemical_formula_weight         351.39
_chemical_absolute_configuration rm
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'I 1 2 1'
_space_group_name_Hall           'I 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   24.5330(2)
_cell_length_b                   5.04577(4)
_cell_length_c                   30.1674(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.5159(10)
_cell_angle_gamma                90
_cell_volume                     3519.81(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    26025
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.7190
_cell_measurement_theta_min      3.1250
_shelx_estimated_absorpt_T_max   0.985
_shelx_estimated_absorpt_T_min   0.654
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 0 -3 0.0110
1 -3 1 0.2262
-1 3 -1 0.3888
3 0 -5 0.0200
-3 0 5 0.0200
3 -1 -5 0.1688
5 0 3 0.0110

_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            33288
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.880
_diffrn_reflns_theta_min         3.108
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -114.00 -27.00   0.50    2.99    --  -49.96 -77.00  30.00  174
  2  ω    -26.00  25.00   0.50    2.99    --  -49.96  19.00  60.00  102
  3  ω    -26.00  25.00   0.50    2.99    --  -49.96  19.00  90.00  102
  4  ω    -43.00 -11.00   0.50   11.97    --  -86.25  38.00   0.00   64
  5  ω    -43.00 -11.00   0.50   11.97    --  -86.25  38.00  60.00   64
  6  ω    -43.00 -11.00   0.50   11.97    --  -86.25  38.00  90.00   64
  7  ω    -43.00 -11.00   0.50   11.97    --  -86.25  38.00  30.00   64
  8  ω    -87.00 -15.00   0.50   11.97    --  -86.25 125.00 -60.00  144
  9  ω    -65.00  21.00   0.50    2.99    --  -49.96  57.00-180.00  172
 10  ω    -43.00 -11.00   0.50   11.97    --  -86.25  38.00-180.00   64
 11  ω    -43.00 -11.00   0.50   11.97    --  -86.25  38.00-150.00   64
 12  ω   -114.00 -27.00   0.50    2.99    --  -49.96 -77.00 -90.00  174
 13  ω   -114.00 -27.00   0.50    2.99    --  -49.96 -77.00  90.00  174
 14  ω   -114.00 -33.00   0.50    2.99    --  -49.96 -77.00 -60.00  162
 15  ω   -114.00 -27.00   0.50    2.99    --  -49.96 -77.00-180.00  174
 16  ω   -114.00 -27.00   0.50    2.99    --  -49.96 -77.00-150.00  174
 17  ω    -25.00  26.00   0.50    2.99    --   49.96 -19.00-120.00  102
 18  ω     37.00  66.00   0.50   11.97    --  107.75 -57.00-150.00   58
 19  ω     37.00  66.00   0.50   11.97    --  107.75 -57.00-180.00   58
 20  ω     37.00  66.00   0.50   11.97    --  107.75 -57.00-120.00   58
 21  ω     43.00 105.00   0.50   11.97    --  107.75 -77.00-180.00  124
 22  ω     97.00 178.00   0.50   11.97    --  107.75  19.00 -60.00  162
 23  ω     97.00 178.00   0.50   11.97    --  107.75  38.00-180.00  162
 24  ω     97.00 178.00   0.50   11.97    --  107.75  19.00 -30.00  162
 25  ω     97.00 178.00   0.50   11.97    --  107.75  38.00 -90.00  162
 26  ω     93.00 178.00   0.50   11.97    --  107.75  57.00   0.00  170
 27  ω     36.00 112.00   0.50   11.97    --  107.75-125.00 150.00  152
 28  ω     43.00 105.00   0.50   11.97    --  107.75 -77.00  30.00  124
 29  ω     37.00  66.00   0.50   11.97    --  107.75 -57.00 150.00   58
 30  ω     43.00 105.00   0.50   11.97    --  107.75 -77.00 120.00  124
 31  ω     37.00  66.00   0.50   11.97    --  107.75 -57.00  30.00   58
 32  ω     37.00  66.00   0.50   11.97    --  107.75 -57.00   0.00   58
 33  ω     37.00  66.00   0.50   11.97    --  107.75 -57.00  60.00   58
 34  ω     37.00  66.00   0.50   11.97    --  107.75 -57.00 120.00   58
 35  ω    -25.00  43.00   0.50    2.99    --   49.96 -38.00  90.00  136
 36  ω   -151.00 -64.00   0.50   11.97    --  -86.25 -77.00  30.00  174
 37  ω   -157.00 -71.00   0.50   11.97    --  -86.25 -57.00  30.00  172
 38  ω   -157.00 -71.00   0.50   11.97    --  -86.25 -57.00 -30.00  172
 39  ω   -161.00 -75.00   0.50   11.97    --  -86.25 -19.00   0.00  172
 40  ω   -157.00 -71.00   0.50   11.97    --  -86.25 -57.00 103.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.890
_reflns_number_gt                6882
_reflns_number_total             7143
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details 
;
 Flack x determined using 2826 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         7143
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0254
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0369P)²+1.1311P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0655
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 C3A(H3A), C3(H3), C5(H5), C11(H11), C5A(H5A), C11A(H11A)
1.b Secondary CH2 refined with riding coordinates:
 C10(H10C,H10D), C10A(H10A,H10B), C4A(H4AA,H4AB), C4(H4A,H4B), C6A(H6AA,H6AB),
 C7(H7A,H7B), C6(H6A,H6B), C7A(H7AA,H7AB)
1.c Aromatic/amide H refined with riding coordinates:
 NA(HA), N(H), C13A(H13A), C15A(H15A), C19A(H19A), C16A(H16A), C22A(H22A),
 C20A(H20A), C13(H13), C14A(H14A), C22(H22), C21A(H21A), C14(H14), C16(H16),
 C21(H21), C19(H19), C15(H15), C20(H20)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O4A O 0.76715(5) 0.9945(2) 0.53775(4) 0.0187(2) Uani 1 1 d . . . . .
O4 O 0.47079(4) 0.1775(2) 0.70451(4) 0.0162(2) Uani 1 1 d . . . . .
O3A O 0.76366(5) 0.6742(2) 0.58954(4) 0.0235(3) Uani 1 1 d . . . . .
O1 O 0.57763(5) 0.7062(3) 0.59187(4) 0.0264(3) Uani 1 1 d . . . . .
O1A O 0.69972(5) 0.8206(2) 0.68083(4) 0.0234(3) Uani 1 1 d . . . . .
O3 O 0.48917(5) -0.0963(2) 0.65145(4) 0.0217(2) Uani 1 1 d . . . . .
O2A O 0.67118(5) 1.0088(3) 0.60952(4) 0.0249(3) Uani 1 1 d . . . . .
O2 O 0.60951(5) 0.4955(3) 0.66080(4) 0.0301(3) Uani 1 1 d . . . . .
NA N 0.77887(6) 1.1047(3) 0.61194(4) 0.0171(3) Uani 1 1 d . . . . .
HA H 0.789396 1.263046 0.605586 0.084(11) Uiso 1 1 calc R . . . .
N N 0.49895(6) 0.3522(3) 0.64839(5) 0.0169(3) Uani 1 1 d . . . . .
H H 0.495107 0.502096 0.661960 0.023(5) Uiso 1 1 calc R . . . .
C9 C 0.48717(6) 0.1258(3) 0.66656(5) 0.0150(3) Uani 1 1 d . . . . .
C9A C 0.76945(6) 0.9055(3) 0.58070(5) 0.0166(3) Uani 1 1 d . . . . .
C8A C 0.70986(7) 0.9483(3) 0.64958(5) 0.0179(3) Uani 1 1 d . . . . .
C17A C 0.82897(7) 0.7053(3) 0.43162(5) 0.0172(3) Uani 1 1 d . . . . .
C8 C 0.57160(7) 0.5400(3) 0.61961(5) 0.0181(3) Uani 1 1 d . . . . .
C18A C 0.77331(7) 0.5860(3) 0.40427(5) 0.0168(3) Uani 1 1 d . . . . .
C23A C 0.72969(7) 0.7074(3) 0.41741(5) 0.0177(3) Uani 1 1 d . . . . .
C12A C 0.81914(7) 0.9002(3) 0.46123(5) 0.0174(3) Uani 1 1 d . . . . .
C12 C 0.39001(7) -0.1562(3) 0.77454(6) 0.0188(3) Uani 1 1 d . . . . .
C10 C 0.44334(7) -0.0418(3) 0.71973(5) 0.0171(3) Uani 1 1 d . . . . .
H10C H 0.470595 -0.192220 0.729813 0.017(4) Uiso 1 1 calc R . . . .
H10D H 0.408962 -0.102051 0.693628 0.015(4) Uiso 1 1 calc R . . . .
C3A C 0.77094(7) 1.0478(3) 0.65683(5) 0.0173(3) Uani 1 1 d . . . . .
H3A H 0.798794 0.905038 0.672950 0.013(4) Uiso 1 1 calc R . . . .
C3 C 0.51772(7) 0.3643(3) 0.60755(5) 0.0178(3) Uani 1 1 d . . . . .
H3 H 0.528513 0.181459 0.600729 0.017(4) Uiso 1 1 calc R . . . .
C10A C 0.74578(7) 0.7999(3) 0.50075(5) 0.0191(3) Uani 1 1 d . . . . .
H10A H 0.704038 0.768332 0.494460 0.018(5) Uiso 1 1 calc R . . . .
H10B H 0.766562 0.630059 0.510396 0.020(5) Uiso 1 1 calc R . . . .
C13A C 0.86460(7) 1.0508(4) 0.48989(5) 0.0210(3) Uani 1 1 d . . . . .
H13A H 0.858152 1.183622 0.509905 0.024(5) Uiso 1 1 calc R . . . .
C5 C 0.41851(7) 0.2865(4) 0.54587(6) 0.0218(3) Uani 1 1 d . . . . .
H5 H 0.399985 0.234278 0.569484 0.034(6) Uiso 1 1 calc R . . . .
C4A C 0.78391(7) 1.2929(3) 0.68861(6) 0.0199(3) Uani 1 1 d . . . . .
H4AA H 0.755710 1.433860 0.673638 0.032(6) Uiso 1 1 calc R . . . .
H4AB H 0.778971 1.247236 0.718965 0.015(4) Uiso 1 1 calc R . . . .
C18 C 0.47057(8) -0.0781(4) 0.84098(6) 0.0231(3) Uani 1 1 d . . . . .
C11 C 0.42549(7) 0.0558(3) 0.76078(5) 0.0176(3) Uani 1 1 d . . . . .
H11 H 0.402593 0.223165 0.751966 0.017(5) Uiso 1 1 calc R . . . .
C15A C 0.92983(7) 0.8045(4) 0.45984(6) 0.0241(4) Uani 1 1 d . . . . .
H15A H 0.968035 0.772169 0.459983 0.026(5) Uiso 1 1 calc R . . . .
C23 C 0.47567(7) 0.0948(3) 0.80618(5) 0.0202(3) Uani 1 1 d . . . . .
C19A C 0.76025(7) 0.3879(3) 0.37010(6) 0.0212(3) Uani 1 1 d . . . . .
H19A H 0.789860 0.305388 0.361241 0.028(5) Uiso 1 1 calc R . . . .
C16A C 0.88444(7) 0.6544(4) 0.43104(5) 0.0206(3) Uani 1 1 d . . . . .
H16A H 0.891071 0.519976 0.411383 0.021(5) Uiso 1 1 calc R . . . .
C5A C 0.84429(7) 1.3970(3) 0.69780(6) 0.0214(3) Uani 1 1 d . . . . .
H5A H 0.853059 1.458348 0.669388 0.027(5) Uiso 1 1 calc R . . . .
C22A C 0.67231(7) 0.6334(4) 0.39647(6) 0.0217(3) Uani 1 1 d . . . . .
H22A H 0.642624 0.715448 0.405301 0.019(5) Uiso 1 1 calc R . . . .
C20A C 0.70278(8) 0.3146(4) 0.34938(6) 0.0244(4) Uani 1 1 d . . . . .
H20A H 0.692995 0.179597 0.326101 0.034(6) Uiso 1 1 calc R . . . .
C4 C 0.47012(7) 0.4680(3) 0.56381(5) 0.0202(3) Uani 1 1 d . . . . .
H4A H 0.456857 0.642420 0.571300 0.026(5) Uiso 1 1 calc R . . . .
H4B H 0.486750 0.495650 0.538448 0.019(5) Uiso 1 1 calc R . . . .
C13 C 0.33829(7) -0.2720(3) 0.74768(6) 0.0221(3) Uani 1 1 d . . . . .
H13 H 0.319643 -0.218704 0.716010 0.026(5) Uiso 1 1 calc R . . . .
C11A C 0.75550(7) 0.9049(3) 0.45659(5) 0.0176(3) Uani 1 1 d . . . . .
H11A H 0.738384 1.085419 0.448013 0.027(5) Uiso 1 1 calc R . . . .
C14A C 0.92009(7) 1.0022(4) 0.48858(6) 0.0241(4) Uani 1 1 d . . . . .
H14A H 0.951657 1.105474 0.507550 0.030(5) Uiso 1 1 calc R . . . .
C17 C 0.41764(7) -0.2343(3) 0.82119(6) 0.0221(3) Uani 1 1 d . . . . .
C22 C 0.52159(7) 0.2718(4) 0.81613(6) 0.0247(4) Uani 1 1 d . . . . .
H22 H 0.524998 0.389740 0.792648 0.033(6) Uiso 1 1 calc R . . . .
C21A C 0.65919(7) 0.4359(4) 0.36216(6) 0.0246(4) Uani 1 1 d . . . . .
H21A H 0.620113 0.383474 0.347338 0.029(5) Uiso 1 1 calc R . . . .
C6A C 0.87393(8) 1.5485(4) 0.74231(6) 0.0268(4) Uani 1 1 d . . . . .
H6AA H 0.898761 1.699903 0.740511 0.030(5) Uiso 1 1 calc R . . . .
H6AB H 0.852898 1.571018 0.764933 0.034(6) Uiso 1 1 calc R . . . .
C14 C 0.31395(8) -0.4688(4) 0.76793(7) 0.0257(4) Uani 1 1 d . . . . .
H14 H 0.278328 -0.548779 0.750057 0.033(6) Uiso 1 1 calc R . . . .
C7 C 0.37773(8) 0.3227(4) 0.49620(6) 0.0276(4) Uani 1 1 d . . . . .
H7A H 0.335867 0.298293 0.490354 0.027(5) Uiso 1 1 calc R . . . .
H7B H 0.387367 0.460287 0.476619 0.032(6) Uiso 1 1 calc R . . . .
C16 C 0.39359(9) -0.4322(4) 0.84115(6) 0.0285(4) Uani 1 1 d . . . . .
H16 H 0.412365 -0.487004 0.872719 0.030(5) Uiso 1 1 calc R . . . .
C21 C 0.56250(8) 0.2733(4) 0.86106(7) 0.0305(4) Uani 1 1 d . . . . .
H21 H 0.594101 0.393285 0.868259 0.036(6) Uiso 1 1 calc R . . . .
C19 C 0.51176(9) -0.0757(4) 0.88585(6) 0.0325(4) Uani 1 1 d . . . . .
H19 H 0.508500 -0.193124 0.909446 0.037(6) Uiso 1 1 calc R . . . .
C15 C 0.34188(9) -0.5474(4) 0.81423(7) 0.0291(4) Uani 1 1 d . . . . .
H15 H 0.325203 -0.682313 0.827570 0.029(5) Uiso 1 1 calc R . . . .
C6 C 0.41585(8) 0.0826(4) 0.50891(6) 0.0278(4) Uani 1 1 d . . . . .
H6A H 0.448878 0.072369 0.497069 0.039(6) Uiso 1 1 calc R . . . .
H6B H 0.397394 -0.089578 0.510800 0.049(7) Uiso 1 1 calc R . . . .
C7A C 0.89412(8) 1.2763(4) 0.73593(7) 0.0336(4) Uani 1 1 d . . . . .
H7AA H 0.885593 1.130859 0.754661 0.045(7) Uiso 1 1 calc R . . . .
H7AB H 0.931445 1.259718 0.730245 0.040(6) Uiso 1 1 calc R . . . .
C20 C 0.55767(9) 0.1010(4) 0.89557(7) 0.0362(5) Uani 1 1 d . . . . .
H20 H 0.586031 0.104260 0.926049 0.045(7) Uiso 1 1 calc R . . . .
H2A H 0.6365(13) 0.925(7) 0.6056(10) 0.063(9) Uiso 1 1 d . . . . .
H2 H 0.6418(13) 0.607(7) 0.6664(10) 0.065(9) Uiso 1 1 d . . . . .


_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
O4A C9A 1.3544(19) . ?
O4A C10A 1.4470(19) . ?
O4 C9 1.3593(18) . ?
O4 C10 1.4475(18) . ?
O3A C9A 1.216(2) . ?
O1 C8 1.228(2) . ?
O1A C8A 1.2340(19) . ?
O3 C9 1.217(2) . ?
O2A C8A 1.299(2) . ?
O2A H2A 0.92(3) . ?
O2 C8 1.299(2) . ?
O2 H2 0.94(3) . ?
NA HA 0.8800 . ?
NA C9A 1.344(2) . ?
NA C3A 1.4597(19) . ?
N H 0.8800 . ?
N C9 1.339(2) . ?
N C3 1.4538(19) . ?
C8A C3A 1.525(2) . ?
C17A C18A 1.468(2) . ?
C17A C12A 1.402(2) . ?
C17A C16A 1.391(2) . ?
C8 C3 1.531(2) . ?
C18A C23A 1.401(2) . ?
C18A C19A 1.394(2) . ?
C23A C22A 1.388(2) . ?
C23A C11A 1.514(2) . ?
C12A C13A 1.387(2) . ?
C12A C11A 1.521(2) . ?
C12 C11 1.522(2) . ?
C12 C13 1.386(2) . ?
C12 C17 1.399(2) . ?
C10 H10C 0.9900 . ?
C10 H10D 0.9900 . ?
C10 C11 1.526(2) . ?
C3A H3A 1.0000 . ?
C3A C4A 1.532(2) . ?
C3 H3 1.0000 . ?
C3 C4 1.533(2) . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
C10A C11A 1.525(2) . ?
C13A H13A 0.9500 . ?
C13A C14A 1.397(2) . ?
C5 H5 1.0000 . ?
C5 C4 1.509(2) . ?
C5 C7 1.509(2) . ?
C5 C6 1.502(2) . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C4A C5A 1.508(2) . ?
C18 C23 1.402(2) . ?
C18 C17 1.465(3) . ?
C18 C19 1.393(2) . ?
C11 H11 1.0000 . ?
C11 C23 1.518(2) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.386(2) . ?
C15A C14A 1.394(3) . ?
C23 C22 1.389(2) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.388(2) . ?
C16A H16A 0.9500 . ?
C5A H5A 1.0000 . ?
C5A C6A 1.504(2) . ?
C5A C7A 1.500(3) . ?
C22A H22A 0.9500 . ?
C22A C21A 1.395(2) . ?
C20A H20A 0.9500 . ?
C20A C21A 1.393(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C13 H13 0.9500 . ?
C13 C14 1.400(2) . ?
C11A H11A 1.0000 . ?
C14A H14A 0.9500 . ?
C17 C16 1.395(2) . ?
C22 H22 0.9500 . ?
C22 C21 1.391(3) . ?
C21A H21A 0.9500 . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C6A C7A 1.494(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.392(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C6 1.500(3) . ?
C16 H16 0.9500 . ?
C16 C15 1.385(3) . ?
C21 H21 0.9500 . ?
C21 C20 1.391(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.389(3) . ?
C15 H15 0.9500 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?
C20 H20 0.9500 . ?

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
C9A O4A C10A 113.68(12) . . ?
C9 O4 C10 114.85(12) . . ?
C8A O2A H2A 111.6(19) . . ?
C8 O2 H2 111.2(18) . . ?
C9A NA HA 121.4 . . ?
C9A NA C3A 117.26(13) . . ?
C3A NA HA 121.4 . . ?
C9 N H 118.1 . . ?
C9 N C3 123.74(13) . . ?
C3 N H 118.1 . . ?
O3 C9 O4 123.53(14) . . ?
O3 C9 N 126.22(14) . . ?
N C9 O4 110.24(13) . . ?
O3A C9A O4A 123.88(14) . . ?
O3A C9A NA 124.71(14) . . ?
NA C9A O4A 111.41(13) . . ?
O1A C8A O2A 124.22(15) . . ?
O1A C8A C3A 120.10(14) . . ?
O2A C8A C3A 115.68(13) . . ?
C12A C17A C18A 108.67(13) . . ?
C16A C17A C18A 130.34(15) . . ?
C16A C17A C12A 120.99(15) . . ?
O1 C8 O2 124.00(15) . . ?
O1 C8 C3 121.62(14) . . ?
O2 C8 C3 114.38(14) . . ?
C23A C18A C17A 108.46(13) . . ?
C19A C18A C17A 130.59(15) . . ?
C19A C18A C23A 120.95(15) . . ?
C18A C23A C11A 110.44(13) . . ?
C22A C23A C18A 120.54(15) . . ?
C22A C23A C11A 128.97(15) . . ?
C17A C12A C11A 110.01(13) . . ?
C13A C12A C17A 120.50(14) . . ?
C13A C12A C11A 129.47(15) . . ?
C13 C12 C11 129.22(15) . . ?
C13 C12 C17 120.70(15) . . ?
C17 C12 C11 110.07(14) . . ?
O4 C10 H10C 110.2 . . ?
O4 C10 H10D 110.2 . . ?
O4 C10 C11 107.51(12) . . ?
H10C C10 H10D 108.5 . . ?
C11 C10 H10C 110.2 . . ?
C11 C10 H10D 110.2 . . ?
NA C3A C8A 111.16(12) . . ?
NA C3A H3A 108.2 . . ?
NA C3A C4A 110.95(13) . . ?
C8A C3A H3A 108.2 . . ?
C8A C3A C4A 110.12(12) . . ?
C4A C3A H3A 108.2 . . ?
N C3 C8 108.40(12) . . ?
N C3 H3 108.4 . . ?
N C3 C4 112.21(13) . . ?
C8 C3 H3 108.4 . . ?
C8 C3 C4 110.86(13) . . ?
C4 C3 H3 108.4 . . ?
O4A C10A H10A 110.0 . . ?
O4A C10A H10B 110.0 . . ?
O4A C10A C11A 108.43(13) . . ?
H10A C10A H10B 108.4 . . ?
C11A C10A H10A 110.0 . . ?
C11A C10A H10B 110.0 . . ?
C12A C13A H13A 120.8 . . ?
C12A C13A C14A 118.32(16) . . ?
C14A C13A H13A 120.8 . . ?
C4 C5 H5 115.5 . . ?
C4 C5 C7 118.76(15) . . ?
C7 C5 H5 115.5 . . ?
C6 C5 H5 115.5 . . ?
C6 C5 C4 120.35(14) . . ?
C6 C5 C7 59.75(12) . . ?
C3A C4A H4AA 109.1 . . ?
C3A C4A H4AB 109.1 . . ?
H4AA C4A H4AB 107.8 . . ?
C5A C4A C3A 112.48(13) . . ?
C5A C4A H4AA 109.1 . . ?
C5A C4A H4AB 109.1 . . ?
C23 C18 C17 108.55(14) . . ?
C19 C18 C23 120.33(17) . . ?
C19 C18 C17 131.10(17) . . ?
C12 C11 C10 109.88(13) . . ?
C12 C11 H11 110.2 . . ?
C10 C11 H11 110.2 . . ?
C23 C11 C12 102.16(13) . . ?
C23 C11 C10 114.07(12) . . ?
C23 C11 H11 110.2 . . ?
C16A C15A H15A 119.6 . . ?
C16A C15A C14A 120.82(15) . . ?
C14A C15A H15A 119.6 . . ?
C18 C23 C11 110.27(14) . . ?
C22 C23 C18 120.44(15) . . ?
C22 C23 C11 129.28(15) . . ?
C18A C19A H19A 120.9 . . ?
C20A C19A C18A 118.17(15) . . ?
C20A C19A H19A 120.9 . . ?
C17A C16A H16A 120.8 . . ?
C15A C16A C17A 118.39(16) . . ?
C15A C16A H16A 120.8 . . ?
C4A C5A H5A 115.4 . . ?
C6A C5A C4A 119.56(14) . . ?
C6A C5A H5A 115.4 . . ?
C7A C5A C4A 119.89(15) . . ?
C7A C5A H5A 115.4 . . ?
C7A C5A C6A 59.66(12) . . ?
C23A C22A H22A 120.7 . . ?
C23A C22A C21A 118.53(15) . . ?
C21A C22A H22A 120.7 . . ?
C19A C20A H20A 119.5 . . ?
C19A C20A C21A 121.09(16) . . ?
C21A C20A H20A 119.5 . . ?
C3 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
C5 C4 C3 114.09(13) . . ?
C5 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C12 C13 H13 120.5 . . ?
C12 C13 C14 118.99(16) . . ?
C14 C13 H13 120.5 . . ?
C23A C11A C12A 102.15(12) . . ?
C23A C11A C10A 107.86(13) . . ?
C23A C11A H11A 111.6 . . ?
C12A C11A C10A 111.69(13) . . ?
C12A C11A H11A 111.6 . . ?
C10A C11A H11A 111.6 . . ?
C13A C14A H14A 119.5 . . ?
C15A C14A C13A 120.96(15) . . ?
C15A C14A H14A 119.5 . . ?
C12 C17 C18 108.91(15) . . ?
C16 C17 C12 120.21(17) . . ?
C16 C17 C18 130.88(16) . . ?
C23 C22 H22 120.6 . . ?
C23 C22 C21 118.87(17) . . ?
C21 C22 H22 120.6 . . ?
C22A C21A H21A 119.6 . . ?
C20A C21A C22A 120.72(15) . . ?
C20A C21A H21A 119.6 . . ?
C5A C6A H6AA 117.8 . . ?
C5A C6A H6AB 117.8 . . ?
H6AA C6A H6AB 114.9 . . ?
C7A C6A C5A 60.02(12) . . ?
C7A C6A H6AA 117.8 . . ?
C7A C6A H6AB 117.8 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.09(17) . . ?
C15 C14 H14 120.0 . . ?
C5 C7 H7A 117.8 . . ?
C5 C7 H7B 117.8 . . ?
H7A C7 H7B 114.9 . . ?
C6 C7 C5 59.91(11) . . ?
C6 C7 H7A 117.8 . . ?
C6 C7 H7B 117.8 . . ?
C17 C16 H16 120.5 . . ?
C15 C16 C17 118.95(17) . . ?
C15 C16 H16 120.5 . . ?
C22 C21 H21 119.6 . . ?
C22 C21 C20 120.77(18) . . ?
C20 C21 H21 119.6 . . ?
C18 C19 H19 120.5 . . ?
C20 C19 C18 119.00(18) . . ?
C20 C19 H19 120.5 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.06(16) . . ?
C16 C15 H15 119.5 . . ?
C5 C6 H6A 117.7 . . ?
C5 C6 H6B 117.7 . . ?
C7 C6 C5 60.35(11) . . ?
C7 C6 H6A 117.7 . . ?
C7 C6 H6B 117.7 . . ?
H6A C6 H6B 114.9 . . ?
C5A C7A H7AA 117.7 . . ?
C5A C7A H7AB 117.7 . . ?
C6A C7A C5A 60.33(12) . . ?
C6A C7A H7AA 117.7 . . ?
C6A C7A H7AB 117.7 . . ?
H7AA C7A H7AB 114.9 . . ?
C21 C20 H20 119.7 . . ?
C19 C20 C21 120.58(17) . . ?
C19 C20 H20 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4A C10A C11A C23A -176.61(12) . . . . ?
O4A C10A C11A C12A 71.92(16) . . . . ?
O4 C10 C11 C12 173.29(12) . . . . ?
O4 C10 C11 C23 -72.71(16) . . . . ?
O1 C8 C3 N -136.40(15) . . . . ?
O1 C8 C3 C4 -12.8(2) . . . . ?
O1A C8A C3A NA 159.16(14) . . . . ?
O1A C8A C3A C4A -77.47(18) . . . . ?
O2A C8A C3A NA -21.24(19) . . . . ?
O2A C8A C3A C4A 102.13(16) . . . . ?
O2 C8 C3 N 44.15(18) . . . . ?
O2 C8 C3 C4 167.73(14) . . . . ?
NA C3A C4A C5A -57.62(17) . . . . ?
N C3 C4 C5 -66.20(18) . . . . ?
C9 O4 C10 C11 -177.35(12) . . . . ?
C9 N C3 C8 -130.09(15) . . . . ?
C9 N C3 C4 107.15(17) . . . . ?
C9A O4A C10A C11A -169.89(13) . . . . ?
C9A NA C3A C8A -57.73(18) . . . . ?
C9A NA C3A C4A 179.37(13) . . . . ?
C8A C3A C4A C5A 178.88(13) . . . . ?
C17A C18A C23A C22A 179.35(14) . . . . ?
C17A C18A C23A C11A -3.16(17) . . . . ?
C17A C18A C19A C20A -179.37(16) . . . . ?
C17A C12A C13A C14A -0.3(2) . . . . ?
C17A C12A C11A C23A -5.16(16) . . . . ?
C17A C12A C11A C10A 109.87(15) . . . . ?
C8 C3 C4 C5 172.44(13) . . . . ?
C18A C17A C12A C13A -177.76(14) . . . . ?
C18A C17A C12A C11A 3.58(17) . . . . ?
C18A C17A C16A C15A 177.83(16) . . . . ?
C18A C23A C22A C21A 0.0(2) . . . . ?
C18A C23A C11A C12A 5.01(16) . . . . ?
C18A C23A C11A C10A -112.80(14) . . . . ?
C18A C19A C20A C21A 0.2(3) . . . . ?
C23A C18A C19A C20A 0.1(2) . . . . ?
C23A C22A C21A C20A 0.3(2) . . . . ?
C12A C17A C18A C23A -0.28(17) . . . . ?
C12A C17A C18A C19A 179.26(16) . . . . ?
C12A C17A C16A C15A -1.2(2) . . . . ?
C12A C13A C14A C15A -1.1(3) . . . . ?
C12 C11 C23 C18 1.63(17) . . . . ?
C12 C11 C23 C22 -177.28(16) . . . . ?
C12 C13 C14 C15 -0.6(2) . . . . ?
C12 C17 C16 C15 -0.6(2) . . . . ?
C10 O4 C9 O3 -13.3(2) . . . . ?
C10 O4 C9 N 165.17(12) . . . . ?
C10 C11 C23 C18 -116.87(15) . . . . ?
C10 C11 C23 C22 64.2(2) . . . . ?
C3A NA C9A O4A 168.07(12) . . . . ?
C3A NA C9A O3A -11.9(2) . . . . ?
C3A C4A C5A C6A -153.23(15) . . . . ?
C3A C4A C5A C7A -83.34(19) . . . . ?
C3 N C9 O4 179.93(13) . . . . ?
C3 N C9 O3 -1.6(2) . . . . ?
C10A O4A C9A O3A 11.7(2) . . . . ?
C10A O4A C9A NA -168.28(12) . . . . ?
C13A C12A C11A C23A 176.33(16) . . . . ?
C13A C12A C11A C10A -68.6(2) . . . . ?
C4A C5A C6A C7A 109.38(18) . . . . ?
C4A C5A C7A C6A -108.84(17) . . . . ?
C18 C23 C22 C21 0.4(2) . . . . ?
C18 C17 C16 C15 179.31(17) . . . . ?
C18 C19 C20 C21 0.0(3) . . . . ?
C11 C12 C13 C14 178.85(15) . . . . ?
C11 C12 C17 C18 1.63(18) . . . . ?
C11 C12 C17 C16 -178.46(15) . . . . ?
C11 C23 C22 C21 179.18(16) . . . . ?
C23 C18 C17 C12 -0.55(18) . . . . ?
C23 C18 C17 C16 179.56(17) . . . . ?
C23 C18 C19 C20 0.3(3) . . . . ?
C23 C22 C21 C20 -0.1(3) . . . . ?
C19A C18A C23A C22A -0.2(2) . . . . ?
C19A C18A C23A C11A 177.25(14) . . . . ?
C19A C20A C21A C22A -0.5(3) . . . . ?
C16A C17A C18A C23A -179.40(16) . . . . ?
C16A C17A C18A C19A 0.1(3) . . . . ?
C16A C17A C12A C13A 1.5(2) . . . . ?
C16A C17A C12A C11A -177.20(14) . . . . ?
C16A C15A C14A C13A 1.4(3) . . . . ?
C22A C23A C11A C12A -177.77(16) . . . . ?
C22A C23A C11A C10A 64.4(2) . . . . ?
C4 C5 C7 C6 110.31(17) . . . . ?
C4 C5 C6 C7 -107.70(18) . . . . ?
C13 C12 C11 C10 -59.4(2) . . . . ?
C13 C12 C11 C23 179.13(16) . . . . ?
C13 C12 C17 C18 -179.36(14) . . . . ?
C13 C12 C17 C16 0.5(2) . . . . ?
C13 C14 C15 C16 0.6(3) . . . . ?
C11A C23A C22A C21A -176.96(16) . . . . ?
C11A C12A C13A C14A 178.08(16) . . . . ?
C14A C15A C16A C17A -0.2(2) . . . . ?
C17 C12 C11 C10 119.46(14) . . . . ?
C17 C12 C11 C23 -1.97(17) . . . . ?
C17 C12 C13 C14 0.1(2) . . . . ?
C17 C18 C23 C11 -0.76(18) . . . . ?
C17 C18 C23 C22 178.26(15) . . . . ?
C17 C18 C19 C20 -178.15(18) . . . . ?
C17 C16 C15 C14 0.0(3) . . . . ?
C22 C21 C20 C19 -0.2(3) . . . . ?
C7 C5 C4 C3 -162.05(15) . . . . ?
C19 C18 C23 C11 -179.51(15) . . . . ?
C19 C18 C23 C22 -0.5(2) . . . . ?
C19 C18 C17 C12 178.02(18) . . . . ?
C19 C18 C17 C16 -1.9(3) . . . . ?
C6 C5 C4 C3 -92.21(18) . . . . ?

_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
- Detector area scaling
- B-factor correction
;
####################################################################### 
# 
# 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_kk2
_database_code_depnum_ccdc_archive 'CCDC 2203893'
loop_
_audit_author_name
_audit_author_address
Fruzinski
;Technical University of Lodz
Poland
;
_audit_update_record             
;
2022-08-28 deposited with the CCDC.	2022-11-04 downloaded from the CCDC.
;
_audit_creation_date             2022-04-22
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'[Ac-b-cyclopropyl-(R,S)-Ala-OH], 2-(cyclopropylmethyl)-2-acetamidopropanedioic acid hydrate'
_chemical_formula_moiety         'C9 H13 N O5, H2 O'
_chemical_formula_sum            'C9 H15 N O6'
_chemical_formula_weight         233.22
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-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                   13.72920(10)
_cell_length_b                   10.90840(10)
_cell_length_c                   14.82920(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2220.87(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      78.806
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.014
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39926
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.806
_diffrn_reflns_theta_min         5.968
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2229
_reflns_number_total             2308
_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 > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.00105(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2308
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0294
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0369P)²+1.1234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0789
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O(HA,HB)
2.b Ternary CH refined with riding coordinates:
 C5(H5A)
2.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C7(H7A,H7B), C6(H6A,H6B)
2.d Aromatic/amide H refined with riding coordinates:
 N(H)
2.e Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
2.f Idealised tetrahedral OH refined as rotating group:
 O3(H3), O5(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O 0.37333(5) 0.83944(7) 0.63025(5) 0.01538(18) Uani 1 1 d . . . . .
H3 H 0.315296 0.848743 0.619097 0.023 Uiso 1 1 calc R U . . .
O1 O 0.48506(5) 0.75164(7) 0.46572(5) 0.01537(18) Uani 1 1 d . . . . .
O5 O 0.45854(5) 0.68598(7) 0.80295(5) 0.01584(18) Uani 1 1 d . . . . .
H5 H 0.470766 0.706966 0.854826 0.024 Uiso 1 1 calc R U . . .
O O 0.19616(6) 0.89277(7) 0.59160(5) 0.01690(18) Uani 1 1 d G . . . .
HA H 0.157732 0.862710 0.630703 0.025 Uiso 1 1 d G U . . .
HB H 0.187362 0.969739 0.595150 0.025 Uiso 1 1 d G U . . .
O2 O 0.33695(5) 0.64083(7) 0.61439(5) 0.01756(18) Uani 1 1 d . . . . .
O4 O 0.58529(6) 0.80773(7) 0.76904(5) 0.01811(19) Uani 1 1 d . . . . .
N N 0.56366(6) 0.78521(8) 0.59614(6) 0.01274(19) Uani 1 1 d . . . . .
H H 0.610551 0.822701 0.622936 0.015 Uiso 1 1 calc R U . . .
C8 C 0.39484(7) 0.72239(9) 0.62754(7) 0.0123(2) Uani 1 1 d . . . . .
C3 C 0.50403(7) 0.70118(9) 0.64885(7) 0.0117(2) Uani 1 1 d . . . . .
C1 C 0.54963(7) 0.80721(9) 0.50879(7) 0.0127(2) Uani 1 1 d . . . . .
C9 C 0.51957(7) 0.73834(9) 0.74798(7) 0.0126(2) Uani 1 1 d . . . . .
C4 C 0.53402(7) 0.56610(9) 0.63592(7) 0.0136(2) Uani 1 1 d . . . . .
H4A H 0.482758 0.513944 0.659453 0.016 Uiso 1 1 calc R U . . .
H4B H 0.539898 0.549544 0.571878 0.016 Uiso 1 1 calc R U . . .
C2 C 0.61360(8) 0.90187(10) 0.46583(7) 0.0169(2) Uani 1 1 d . . . . .
H2A H 0.660674 0.862208 0.427883 0.025 Uiso 1 1 calc R U . . .
H2B H 0.646648 0.947667 0.511878 0.025 Uiso 1 1 calc R U . . .
H2C H 0.574484 0.956420 0.430204 0.025 Uiso 1 1 calc R U . . .
C5 C 0.62891(7) 0.53260(10) 0.68161(7) 0.0157(2) Uani 1 1 d . . . . .
H5A H 0.627263 0.535388 0.747647 0.019 Uiso 1 1 calc R U . . .
C7 C 0.69107(8) 0.43211(11) 0.64256(8) 0.0198(2) Uani 1 1 d . . . . .
H7A H 0.670297 0.395330 0.586196 0.024 Uiso 1 1 calc R U . . .
H7B H 0.722754 0.376338 0.684213 0.024 Uiso 1 1 calc R U . . .
C6 C 0.72616(8) 0.56348(11) 0.64024(8) 0.0205(2) Uani 1 1 d . . . . .
H6A H 0.778787 0.586289 0.680530 0.025 Uiso 1 1 calc R U . . .
H6B H 0.726325 0.605284 0.582502 0.025 Uiso 1 1 calc R U . . .


_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
O3 H3 0.8200 . ?
O3 C8 1.3111(13) . ?
O1 C1 1.2495(13) . ?
O5 H5 0.8200 . ?
O5 C9 1.3012(13) . ?
O HA 0.8498 . ?
O HB 0.8499 . ?
O2 C8 1.2089(13) . ?
O4 C9 1.2184(13) . ?
N H 0.8600 . ?
N C3 1.4566(13) . ?
N C1 1.3314(13) . ?
C8 C3 1.5493(14) . ?
C3 C9 1.5397(14) . ?
C3 C4 1.5419(14) . ?
C1 C2 1.4978(14) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.5132(14) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C5 H5A 0.9800 . ?
C5 C7 1.5051(15) . ?
C5 C6 1.5076(15) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C6 1.5123(16) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 O3 H3 109.5 . . ?
C9 O5 H5 109.5 . . ?
HA O HB 104.5 . . ?
C3 N H 118.2 . . ?
C1 N H 118.2 . . ?
C1 N C3 123.66(9) . . ?
O3 C8 C3 110.93(9) . . ?
O2 C8 O3 124.99(10) . . ?
O2 C8 C3 123.99(9) . . ?
N C3 C8 109.90(8) . . ?
N C3 C9 105.59(8) . . ?
N C3 C4 112.61(8) . . ?
C9 C3 C8 106.83(8) . . ?
C9 C3 C4 109.47(8) . . ?
C4 C3 C8 112.07(8) . . ?
O1 C1 N 120.83(9) . . ?
O1 C1 C2 122.21(9) . . ?
N C1 C2 116.95(9) . . ?
O5 C9 C3 113.16(8) . . ?
O4 C9 O5 126.08(10) . . ?
O4 C9 C3 120.73(9) . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C5 C4 C3 113.89(9) . . ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C5 H5A 114.8 . . ?
C7 C5 C4 119.45(9) . . ?
C7 C5 H5A 114.8 . . ?
C7 C5 C6 60.26(7) . . ?
C6 C5 C4 121.75(9) . . ?
C6 C5 H5A 114.8 . . ?
C5 C7 H7A 117.8 . . ?
C5 C7 H7B 117.8 . . ?
C5 C7 C6 59.95(7) . . ?
H7A C7 H7B 114.9 . . ?
C6 C7 H7A 117.8 . . ?
C6 C7 H7B 117.8 . . ?
C5 C6 C7 59.79(7) . . ?
C5 C6 H6A 117.8 . . ?
C5 C6 H6B 117.8 . . ?
C7 C6 H6A 117.8 . . ?
C7 C6 H6B 117.8 . . ?
H6A C6 H6B 114.9 . . ?

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
O3 C8 C3 N -47.67(11) . . . . ?
O3 C8 C3 C9 66.41(10) . . . . ?
O3 C8 C3 C4 -173.69(8) . . . . ?
O2 C8 C3 N 135.48(10) . . . . ?
O2 C8 C3 C9 -110.44(11) . . . . ?
O2 C8 C3 C4 9.46(14) . . . . ?
N C3 C9 O5 168.82(8) . . . . ?
N C3 C9 O4 -12.95(13) . . . . ?
N C3 C4 C5 72.96(11) . . . . ?
C8 C3 C9 O5 51.85(11) . . . . ?
C8 C3 C9 O4 -129.92(10) . . . . ?
C8 C3 C4 C5 -162.51(8) . . . . ?
C3 N C1 O1 -2.85(15) . . . . ?
C3 N C1 C2 176.41(9) . . . . ?
C3 C4 C5 C7 -150.97(9) . . . . ?
C3 C4 C5 C6 -79.66(12) . . . . ?
C1 N C3 C8 -44.94(13) . . . . ?
C1 N C3 C9 -159.81(9) . . . . ?
C1 N C3 C4 80.77(12) . . . . ?
C9 C3 C4 C5 -44.17(11) . . . . ?
C4 C3 C9 O5 -69.71(11) . . . . ?
C4 C3 C9 O4 108.52(10) . . . . ?
C4 C5 C7 C6 111.93(11) . . . . ?
C4 C5 C6 C7 -108.21(11) . . . . ?

_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_kk_big
_database_code_depnum_ccdc_archive 'CCDC 2203891'
loop_
_audit_author_name
_audit_author_address
Fruzinski
;Technical University of Lodz
Poland
;
_audit_update_record             
;
2022-08-28 deposited with the CCDC.	2022-11-04 downloaded from the CCDC.
;
_audit_creation_date             2022-04-22
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '2-acetamido-3-cyclopropylpropanoic acid'
_chemical_formula_moiety         'C8 H13 N O3'
_chemical_formula_sum            'C8 H13 N O3'
_chemical_formula_weight         171.19
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   14.66220(10)
_cell_length_b                   11.42930(10)
_cell_length_c                   21.61680(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.6010(10)
_cell_angle_gamma                90
_cell_volume                     3622.32(4)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    84697
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      78.7620
_cell_measurement_theta_min      3.6860
_shelx_estimated_absorpt_T_max   0.856
_shelx_estimated_absorpt_T_min   0.608
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1472
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 5 0.1071
6 -1 -11 0.1605
0 -5 4 0.1452
-3 3 -5 0.1428
2 4 5 0.2872
2 -1 -5 0.1216
0 -2 -5 0.1271
-2 -4 -5 0.2005
-5 -3 3 0.2696
5 -2 5 0.1208
-1 -1 14 0.1017
0 -1 14 0.0918
0 1 -14 0.1045
5 3 10 0.2282
-6 6 1 0.1328
1 -7 0 0.1347
9 -3 -1 0.1485
8 -4 -1 0.1288
2 7 0 0.3387

_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            119641
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.950
_diffrn_reflns_theta_min         3.014
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -124.00 -39.00   0.50    0.10    --  -49.71 -38.00 -90.00  170
  2  ω    -26.00  26.00   0.50    0.10    --  -49.71  19.00 -90.00  104
  3  ω   -114.00 -27.00   0.50    0.10    --  -49.71 -77.00  30.00  174
  4  ω    -26.00  26.00   0.50    0.10    --  -49.71  19.00-150.00  104
  5  ω   -121.00 -35.00   0.50    0.10    --  -49.71 -57.00  60.00  172
  6  ω    -43.00  25.00   0.50    0.10    --  -49.71  38.00 120.00  136
  7  ω    -26.00  26.00   0.50    0.10    --  -49.71  19.00  90.00  104
  8  ω     62.00 120.00   0.50    0.10    --   49.71 178.00 -30.00  116
  9  ω    -25.00  26.00   0.50    0.10    --   49.71 -19.00 -60.00  102
 10  ω    -43.00 -11.00   0.50    0.13    --  -86.25  38.00 -90.00   64
 11  ω   -161.00 -75.00   0.50    0.13    --  -86.25 -19.00 -30.00  172
 12  ω    -43.00 -11.00   0.50    0.13    --  -86.25  38.00  90.00   64
 13  ω   -151.00 -64.00   0.50    0.13    --  -86.25 -77.00  30.00  174
 14  ω   -151.00 -64.00   0.50    0.13    --  -86.25 -77.00  60.00  174
 15  ω    -43.00 -11.00   0.50    0.13    --  -86.25  38.00  60.00   64
 16  ω   -105.00 -22.00   0.50    0.13    --  -86.25  77.00 -90.00  166
 17  ω    -43.00 -11.00   0.50    0.13    --  -86.25  38.00  30.00   64
 18  ω    -43.00 -11.00   0.50    0.13    --  -86.25  38.00-180.00   64
 19  ω    -43.00 -11.00   0.50    0.13    --  -86.25  38.00   0.00   64
 20  ω   -157.00 -71.00   0.50    0.13    --  -86.25 -57.00 -30.00  172
 21  ω    -66.00 -15.00   0.50    0.13    --  -86.25  57.00-150.00  102
 22  ω     37.00  66.00   0.50    0.13    --  107.75 -57.00 150.00   58
 23  ω     97.00 178.00   0.50    0.13    --  107.75  19.00-120.00  162
 24  ω     37.00  66.00   0.50    0.13    --  107.75 -57.00-150.00   58
 25  ω     93.00 178.00   0.50    0.13    --  107.75  57.00 -30.00  170
 26  ω     37.00  66.00   0.50    0.13    --  107.75 -57.00 -30.00   58
 27  ω     37.00  66.00   0.50    0.13    --  107.75 -57.00  60.00   58
 28  ω     36.00 112.00   0.50    0.13    --  107.75-125.00-180.00  152
 29  ω     37.00  66.00   0.50    0.13    --  107.75 -57.00   0.00   58
 30  ω     97.00 178.00   0.50    0.13    --  107.75  19.00-180.00  162
 31  ω     97.00 178.00   0.50    0.13    --  107.75  38.00  90.00  162
 32  ω     85.00 172.00   0.50    0.13    --  107.75  77.00   0.00  174
 33  ω     93.00 178.00   0.50    0.13    --  107.75  57.00  60.00  170
 34  ω     43.00 105.00   0.50    0.13    --  107.75 -77.00 150.00  124
 35  ω     37.00  66.00   0.50    0.13    --  107.75 -57.00-180.00   58
 36  ω     97.00 178.00   0.50    0.13    --  107.75  38.00  30.00  162
 37  ω     94.00 178.00   0.50    0.13    --  107.75 125.00  90.00  168
 38  ω     37.00  66.00   0.50    0.13    --  107.75 -57.00-120.00   58
 39  ω     37.00  66.00   0.50    0.13    --  107.75 -57.00  30.00   58
 40  ω   -114.00 -27.00   0.50    0.10    --  -49.71 -77.00-180.00  174
 41  ω   -121.00 -35.00   0.50    0.10    --  -49.71 -57.00-120.00  172
 42  ω   -120.00 -34.00   0.50    0.10    --  -49.71 -59.00 132.00  172
 43  ω     35.00 121.00   0.50    0.10    --   49.71  57.00-120.00  172
 44  ω     27.00 114.00   0.50    0.10    --   49.71  77.00-120.00  174
 45  ω     27.00 114.00   0.50    0.10    --   49.71  77.00 120.00  174
 46  ω     60.00 121.00   0.50    0.10    --   49.71-178.00 150.00  122
 47  ω     27.00 114.00   0.50    0.10    --   49.71  77.00  30.00  174
 48  ω     27.00 114.00   0.50    0.10    --   49.71  77.00 -30.00  174
 49  ω   -151.00 -64.00   0.50    0.13    --  -86.25 -77.00-180.00  174
 50  ω   -151.00 -64.00   0.50    0.13    --  -86.25 -77.00-120.00  174
 51  ω   -151.00 -64.00   0.50    0.13    --  -86.25 -77.00   0.00  174
 52  ω   -151.00 -64.00   0.50    0.13    --  -86.25 -77.00 150.00  174
 53  ω   -157.00 -71.00   0.50    0.13    --  -86.25 -59.00 132.00  172
 54  ω   -151.00 -64.00   0.50    0.13    --  -86.25 -77.00  90.00  174
 55  ω   -151.00 -64.00   0.50    0.13    --  -86.25 -77.00 -60.00  174
 56  ω   -151.00 -64.00   0.50    0.13    --  -86.25 -77.00-150.00  174
 57  ω   -151.00 -64.00   0.50    0.13    --  -86.25 -77.00 -30.00  174
 58  ω   -151.00 -64.00   0.50    0.13    --  -86.25 -77.00 120.00  174
 59  ω   -151.00 -64.00   0.50    0.13    --  -86.25 -77.00 -90.00  174
 60  ω     36.00 112.00   0.50    0.13    --  107.75-125.00 -30.00  152
 61  ω     39.00 107.00   0.50    0.13    --  107.75 -99.00 -30.00  136
 62  ω     39.00 107.00   0.50    0.13    --  107.75 -99.00  30.00  136
 63  ω     36.00 112.00   0.50    0.13    --  107.75-125.00 150.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7387
_reflns_number_total             7734
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.00026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7734
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0353
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0423P)²+1.5271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0931
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3A), C3C(H3CA), C3A(H3AB), C3B(H3BA), C5A(H5A), C5C(H5C), C5(H5), C5B(H5B)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C4C(H4CA,H4CB), C4A(H4AA,H4AB), C4B(H4BA,H4BB), C6B(H6BA,H6BB),
 C7(H7A,H7B), C6C(H6CA,H6CB), C6A(H6AA,H6AB), C6(H6A,H6B), C7B(H7BA,H7BB),
 C7C(H7CA,H7CB), C7A(H7AA,H7AB)
2.c Aromatic/amide H refined with riding coordinates:
 NA(HA), N(H), NB(HB), NC(HC)
2.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C2C(H2CA,H2CB,H2CC), C2B(H2BA,H2BB,H2BC), C2A(H2AA,H2AB,H2AC)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O3C(H3C), O3B(H3B), O3A(H3AA)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.38811(5) 0.09390(6) 0.67628(4) 0.01797(16) Uani 1 1 d . . . . .
O3 O 0.05837(5) 0.19936(6) 0.66622(4) 0.01847(16) Uani 1 1 d . . . . .
H3 H 0.002478 0.185656 0.670344 0.028 Uiso 1 1 calc R U . . .
O2B O 0.68014(5) 0.50240(6) 0.69275(3) 0.01618(15) Uani 1 1 d . . . . .
O3C O 0.55870(5) 0.06613(6) 0.68529(4) 0.01756(15) Uani 1 1 d . . . . .
H3C H 0.502191 0.078164 0.685646 0.026 Uiso 1 1 calc R U . . .
O2A O 0.18072(5) 0.76590(6) 0.68571(3) 0.01781(16) Uani 1 1 d . . . . .
O3B O 0.68955(5) 0.69675(6) 0.67912(4) 0.01875(16) Uani 1 1 d . . . . .
H3B H 0.745265 0.685552 0.686373 0.028 Uiso 1 1 calc R U . . .
O1C O 0.88571(5) 0.17551(6) 0.67123(4) 0.01828(16) Uani 1 1 d . . . . .
O2C O 0.56715(5) 0.26177(6) 0.68769(3) 0.01728(15) Uani 1 1 d . . . . .
O3A O 0.19053(5) 0.57121(6) 0.67450(4) 0.01892(16) Uani 1 1 d . . . . .
H3AA H 0.246879 0.584208 0.676362 0.028 Uiso 1 1 calc R U . . .
O1A O -0.13798(5) 0.67525(6) 0.69220(4) 0.01795(16) Uani 1 1 d . . . . .
O1B O 0.36361(5) 0.59311(6) 0.67091(4) 0.01858(16) Uani 1 1 d . . . . .
O2 O 0.06999(5) 0.00414(6) 0.67262(4) 0.02110(17) Uani 1 1 d . . . . .
NA N -0.00230(5) 0.76340(7) 0.68058(4) 0.01371(17) Uani 1 1 d . . . . .
HA H 0.029213 0.828928 0.681253 0.016 Uiso 1 1 calc R U . . .
N N 0.25218(5) 0.00768(7) 0.66091(4) 0.01430(17) Uani 1 1 d . . . . .
H H 0.220796 -0.057548 0.656846 0.017 Uiso 1 1 calc R U . . .
NB N 0.49912(5) 0.50143(7) 0.66925(4) 0.01413(17) Uani 1 1 d . . . . .
HB H 0.529243 0.435070 0.672436 0.017 Uiso 1 1 calc R U . . .
NC N 0.74800(5) 0.26131(7) 0.66761(4) 0.01398(17) Uani 1 1 d . . . . .
HC H 0.716163 0.326587 0.667634 0.017 Uiso 1 1 calc R U . . .
C1B C 0.40909(6) 0.50156(9) 0.67763(4) 0.01412(19) Uani 1 1 d . . . . .
C8A C 0.14597(6) 0.67091(9) 0.67729(4) 0.01374(19) Uani 1 1 d . . . . .
C8B C 0.64645(6) 0.59558(9) 0.67858(4) 0.01391(19) Uani 1 1 d . . . . .
C1A C -0.09128(6) 0.76667(9) 0.69246(5) 0.01427(19) Uani 1 1 d . . . . .
C8C C 0.60173(6) 0.16625(9) 0.68077(4) 0.01328(19) Uani 1 1 d . . . . .
C3 C 0.20532(6) 0.11962(9) 0.65607(5) 0.01457(19) Uani 1 1 d . . . . .
H3A H 0.228774 0.171681 0.689839 0.017 Uiso 1 1 calc R U . . .
C8 C 0.10374(6) 0.10011(9) 0.66614(5) 0.01489(19) Uani 1 1 d . . . . .
C1C C 0.83880(6) 0.26655(9) 0.67257(4) 0.01381(19) Uani 1 1 d . . . . .
C1 C 0.34198(6) 0.00226(9) 0.67143(4) 0.01399(19) Uani 1 1 d . . . . .
C3C C 0.70068(6) 0.14982(8) 0.66216(5) 0.01417(19) Uani 1 1 d . . . . .
H3CA H 0.730288 0.091644 0.690494 0.017 Uiso 1 1 calc R U . . .
C3A C 0.04403(6) 0.65410(8) 0.66651(5) 0.01409(19) Uani 1 1 d . . . . .
H3AB H 0.021512 0.591710 0.694964 0.017 Uiso 1 1 calc R U . . .
C2 C 0.38496(7) -0.11639(9) 0.67684(5) 0.0160(2) Uani 1 1 d . . . . .
H2A H 0.437799 -0.120754 0.649544 0.024 Uiso 1 1 calc R U . . .
H2B H 0.340416 -0.176349 0.664794 0.024 Uiso 1 1 calc R U . . .
H2C H 0.404759 -0.129618 0.719712 0.024 Uiso 1 1 calc R U . . .
C4 C 0.22251(7) 0.18055(9) 0.59368(5) 0.0188(2) Uani 1 1 d . . . . .
H4A H 0.185240 0.252693 0.591560 0.023 Uiso 1 1 calc R U . . .
H4B H 0.287430 0.203987 0.591944 0.023 Uiso 1 1 calc R U . . .
C3B C 0.54882(6) 0.60818(9) 0.65498(5) 0.0158(2) Uani 1 1 d . . . . .
H3BA H 0.519330 0.675525 0.676506 0.019 Uiso 1 1 calc R U . . .
C4C C 0.70219(7) 0.10227(10) 0.59520(5) 0.0206(2) Uani 1 1 d . . . . .
H4CA H 0.766257 0.095340 0.581666 0.025 Uiso 1 1 calc R U . . .
H4CB H 0.674878 0.023062 0.594414 0.025 Uiso 1 1 calc R U . . .
C2C C 0.88082(7) 0.38583(9) 0.67951(5) 0.0166(2) Uani 1 1 d . . . . .
H2CA H 0.885216 0.406027 0.723505 0.025 Uiso 1 1 calc R U . . .
H2CB H 0.842711 0.443674 0.657985 0.025 Uiso 1 1 calc R U . . .
H2CC H 0.941934 0.385581 0.661587 0.025 Uiso 1 1 calc R U . . .
C2B C 0.36570(7) 0.38809(9) 0.69632(5) 0.0188(2) Uani 1 1 d . . . . .
H2BA H 0.358267 0.386664 0.741318 0.028 Uiso 1 1 calc R U . . .
H2BB H 0.404672 0.322793 0.683772 0.028 Uiso 1 1 calc R U . . .
H2BC H 0.305854 0.380779 0.676081 0.028 Uiso 1 1 calc R U . . .
C2A C -0.13211(7) 0.88370(9) 0.70725(5) 0.0204(2) Uani 1 1 d . . . . .
H2AA H -0.192658 0.889754 0.687890 0.031 Uiso 1 1 calc R U . . .
H2AB H -0.092730 0.945852 0.691340 0.031 Uiso 1 1 calc R U . . .
H2AC H -0.137584 0.891899 0.752189 0.031 Uiso 1 1 calc R U . . .
C4A C 0.02639(7) 0.61567(10) 0.59899(5) 0.0198(2) Uani 1 1 d . . . . .
H4AA H 0.057586 0.540208 0.591616 0.024 Uiso 1 1 calc R U . . .
H4AB H -0.039860 0.603184 0.592616 0.024 Uiso 1 1 calc R U . . .
C4B C 0.55016(7) 0.63288(10) 0.58481(5) 0.0232(2) Uani 1 1 d . . . . .
H4BA H 0.486592 0.639100 0.569271 0.028 Uiso 1 1 calc R U . . .
H4BB H 0.580384 0.709069 0.577648 0.028 Uiso 1 1 calc R U . . .
C5A C 0.05940(8) 0.70418(11) 0.55291(5) 0.0260(2) Uani 1 1 d . . . . .
H5A H 0.030517 0.783212 0.555915 0.031 Uiso 1 1 calc R U . . .
C5C C 0.65081(8) 0.17981(12) 0.55058(5) 0.0262(2) Uani 1 1 d . . . . .
H5C H 0.673547 0.262192 0.548478 0.031 Uiso 1 1 calc R U . . .
C5 C 0.20047(8) 0.10584(11) 0.53814(5) 0.0263(2) Uani 1 1 d . . . . .
H5 H 0.241177 0.036524 0.532574 0.032 Uiso 1 1 calc R U . . .
C5B C 0.59894(8) 0.53968(11) 0.54860(5) 0.0264(3) Uani 1 1 d . . . . .
H5B H 0.572060 0.459483 0.551503 0.032 Uiso 1 1 calc R U . . .
C6B C 0.70124(8) 0.54361(12) 0.54283(5) 0.0301(3) Uani 1 1 d . . . . .
H6BA H 0.733952 0.610103 0.562278 0.036 Uiso 1 1 calc R U . . .
H6BB H 0.734693 0.468370 0.543724 0.036 Uiso 1 1 calc R U . . .
C7 C 0.16784(9) 0.16209(13) 0.47911(6) 0.0349(3) Uani 1 1 d . . . . .
H7A H 0.189987 0.129343 0.439621 0.042 Uiso 1 1 calc R U . . .
H7B H 0.158518 0.247883 0.479130 0.042 Uiso 1 1 calc R U . . .
C6C C 0.54932(8) 0.16641(13) 0.54099(6) 0.0326(3) Uani 1 1 d . . . . .
H6CA H 0.518194 0.102878 0.563651 0.039 Uiso 1 1 calc R U . . .
H6CB H 0.512719 0.238431 0.535146 0.039 Uiso 1 1 calc R U . . .
C6A C 0.15724(9) 0.70412(14) 0.53266(6) 0.0362(3) Uani 1 1 d . . . . .
H6AA H 0.198128 0.643178 0.549986 0.043 Uiso 1 1 calc R U . . .
H6AB H 0.186663 0.780705 0.525149 0.043 Uiso 1 1 calc R U . . .
C6 C 0.10387(10) 0.08863(13) 0.51662(6) 0.0367(3) Uani 1 1 d . . . . .
H6A H 0.055214 0.129320 0.539628 0.044 Uiso 1 1 calc R U . . .
H6B H 0.086679 0.010799 0.500125 0.044 Uiso 1 1 calc R U . . .
C7B C 0.64172(9) 0.56886(16) 0.48741(6) 0.0403(3) Uani 1 1 d . . . . .
H7BA H 0.638641 0.509116 0.454293 0.048 Uiso 1 1 calc R U . . .
H7BB H 0.637900 0.650849 0.472848 0.048 Uiso 1 1 calc R U . . .
C7C C 0.61346(10) 0.13240(17) 0.49050(6) 0.0445(4) Uani 1 1 d . . . . .
H7CA H 0.616260 0.183475 0.453581 0.053 Uiso 1 1 calc R U . . .
H7CB H 0.621734 0.047941 0.482082 0.053 Uiso 1 1 calc R U . . .
C7A C 0.08303(10) 0.66573(15) 0.48832(6) 0.0421(4) Uani 1 1 d . . . . .
H7AA H 0.066991 0.718845 0.453705 0.051 Uiso 1 1 calc R U . . .
H7AB H 0.078457 0.581298 0.478546 0.051 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.2505(12) . ?
O3 H3 0.8400 . ?
O3 C8 1.3151(12) . ?
O2B C8B 1.2120(12) . ?
O3C H3C 0.8400 . ?
O3C C8C 1.3109(12) . ?
O2A C8A 1.2122(12) . ?
O3B H3B 0.8400 . ?
O3B C8B 1.3177(12) . ?
O1C C1C 1.2478(12) . ?
O2C C8C 1.2136(12) . ?
O3A H3AA 0.8400 . ?
O3A C8A 1.3152(12) . ?
O1A C1A 1.2492(12) . ?
O1B C1B 1.2483(12) . ?
O2 C8 1.2120(12) . ?
NA HA 0.8800 . ?
NA C1A 1.3329(12) . ?
NA C3A 1.4557(12) . ?
N H 0.8800 . ?
N C3 1.4556(12) . ?
N C1 1.3352(12) . ?
NB HB 0.8800 . ?
NB C1B 1.3343(12) . ?
NB C3B 1.4559(12) . ?
NC HC 0.8800 . ?
NC C1C 1.3360(12) . ?
NC C3C 1.4551(12) . ?
C1B C2B 1.5017(13) . ?
C8A C3A 1.5226(13) . ?
C8B C3B 1.5215(13) . ?
C1A C2A 1.5013(14) . ?
C8C C3C 1.5212(13) . ?
C3 H3A 1.0000 . ?
C3 C8 1.5239(13) . ?
C3 C4 1.5408(14) . ?
C1C C2C 1.5029(13) . ?
C1 C2 1.4994(13) . ?
C3C H3CA 1.0000 . ?
C3C C4C 1.5466(14) . ?
C3A H3AB 1.0000 . ?
C3A C4A 1.5434(14) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.5055(16) . ?
C3B H3BA 1.0000 . ?
C3B C4B 1.5432(15) . ?
C4C H4CA 0.9900 . ?
C4C H4CB 0.9900 . ?
C4C C5C 1.5060(16) . ?
C2C H2CA 0.9800 . ?
C2C H2CB 0.9800 . ?
C2C H2CC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C4A C5A 1.5034(16) . ?
C4B H4BA 0.9900 . ?
C4B H4BB 0.9900 . ?
C4B C5B 1.5068(18) . ?
C5A H5A 1.0000 . ?
C5A C6A 1.5042(17) . ?
C5A C7A 1.5075(16) . ?
C5C H5C 1.0000 . ?
C5C C6C 1.5081(16) . ?
C5C C7C 1.5050(17) . ?
C5 H5 1.0000 . ?
C5 C7 1.5025(16) . ?
C5 C6 1.4991(17) . ?
C5B H5B 1.0000 . ?
C5B C6B 1.5071(16) . ?
C5B C7B 1.5072(16) . ?
C6B H6BA 0.9900 . ?
C6B H6BB 0.9900 . ?
C6B C7B 1.5027(18) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C6 1.503(2) . ?
C6C H6CA 0.9900 . ?
C6C H6CB 0.9900 . ?
C6C C7C 1.4995(18) . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C6A C7A 1.508(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7B H7BA 0.9900 . ?
C7B H7BB 0.9900 . ?
C7C H7CA 0.9900 . ?
C7C H7CB 0.9900 . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?

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
C8 O3 H3 109.5 . . ?
C8C O3C H3C 109.5 . . ?
C8B O3B H3B 109.5 . . ?
C8A O3A H3AA 109.5 . . ?
C1A NA HA 119.2 . . ?
C1A NA C3A 121.61(8) . . ?
C3A NA HA 119.2 . . ?
C3 N H 119.4 . . ?
C1 N H 119.4 . . ?
C1 N C3 121.13(8) . . ?
C1B NB HB 119.1 . . ?
C1B NB C3B 121.73(8) . . ?
C3B NB HB 119.1 . . ?
C1C NC HC 119.3 . . ?
C1C NC C3C 121.31(8) . . ?
C3C NC HC 119.3 . . ?
O1B C1B NB 120.87(9) . . ?
O1B C1B C2B 121.86(8) . . ?
NB C1B C2B 117.25(8) . . ?
O2A C8A O3A 125.08(9) . . ?
O2A C8A C3A 123.12(9) . . ?
O3A C8A C3A 111.77(8) . . ?
O2B C8B O3B 125.08(9) . . ?
O2B C8B C3B 123.19(9) . . ?
O3B C8B C3B 111.67(8) . . ?
O1A C1A NA 120.88(9) . . ?
O1A C1A C2A 121.77(9) . . ?
NA C1A C2A 117.34(8) . . ?
O3C C8C C3C 111.91(8) . . ?
O2C C8C O3C 125.03(9) . . ?
O2C C8C C3C 122.99(9) . . ?
N C3 H3A 108.2 . . ?
N C3 C8 108.81(8) . . ?
N C3 C4 112.26(8) . . ?
C8 C3 H3A 108.2 . . ?
C8 C3 C4 111.12(8) . . ?
C4 C3 H3A 108.2 . . ?
O3 C8 C3 111.66(8) . . ?
O2 C8 O3 124.99(9) . . ?
O2 C8 C3 123.35(9) . . ?
O1C C1C NC 120.65(9) . . ?
O1C C1C C2C 122.23(8) . . ?
NC C1C C2C 117.12(8) . . ?
O1 C1 N 120.46(9) . . ?
O1 C1 C2 121.63(8) . . ?
N C1 C2 117.91(8) . . ?
NC C3C C8C 109.01(8) . . ?
NC C3C H3CA 109.2 . . ?
NC C3C C4C 111.83(8) . . ?
C8C C3C H3CA 109.2 . . ?
C8C C3C C4C 108.29(8) . . ?
C4C C3C H3CA 109.2 . . ?
NA C3A C8A 108.61(8) . . ?
NA C3A H3AB 109.0 . . ?
NA C3A C4A 111.58(8) . . ?
C8A C3A H3AB 109.0 . . ?
C8A C3A C4A 109.58(8) . . ?
C4A C3A H3AB 109.0 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C5 C4 C3 113.95(9) . . ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
NB C3B C8B 108.71(8) . . ?
NB C3B H3BA 109.1 . . ?
NB C3B C4B 111.91(8) . . ?
C8B C3B H3BA 109.1 . . ?
C8B C3B C4B 108.98(8) . . ?
C4B C3B H3BA 109.1 . . ?
C3C C4C H4CA 109.1 . . ?
C3C C4C H4CB 109.1 . . ?
H4CA C4C H4CB 107.9 . . ?
C5C C4C C3C 112.38(9) . . ?
C5C C4C H4CA 109.1 . . ?
C5C C4C H4CB 109.1 . . ?
C1C C2C H2CA 109.5 . . ?
C1C C2C H2CB 109.5 . . ?
C1C C2C H2CC 109.5 . . ?
H2CA C2C H2CB 109.5 . . ?
H2CA C2C H2CC 109.5 . . ?
H2CB C2C H2CC 109.5 . . ?
C1B C2B H2BA 109.5 . . ?
C1B C2B H2BB 109.5 . . ?
C1B C2B H2BC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
C1A C2A H2AA 109.5 . . ?
C1A C2A H2AB 109.5 . . ?
C1A C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C3A C4A H4AA 109.1 . . ?
C3A C4A H4AB 109.1 . . ?
H4AA C4A H4AB 107.8 . . ?
C5A C4A C3A 112.54(9) . . ?
C5A C4A H4AA 109.1 . . ?
C5A C4A H4AB 109.1 . . ?
C3B C4B H4BA 109.0 . . ?
C3B C4B H4BB 109.0 . . ?
H4BA C4B H4BB 107.8 . . ?
C5B C4B C3B 113.10(9) . . ?
C5B C4B H4BA 109.0 . . ?
C5B C4B H4BB 109.0 . . ?
C4A C5A H5A 115.2 . . ?
C4A C5A C6A 120.47(10) . . ?
C4A C5A C7A 119.75(11) . . ?
C6A C5A H5A 115.2 . . ?
C6A C5A C7A 60.08(9) . . ?
C7A C5A H5A 115.2 . . ?
C4C C5C H5C 114.7 . . ?
C4C C5C C6C 120.96(11) . . ?
C6C C5C H5C 114.7 . . ?
C7C C5C C4C 121.05(12) . . ?
C7C C5C H5C 114.7 . . ?
C7C C5C C6C 59.69(8) . . ?
C4 C5 H5 115.0 . . ?
C7 C5 C4 119.89(11) . . ?
C7 C5 H5 115.0 . . ?
C6 C5 C4 121.07(10) . . ?
C6 C5 H5 115.0 . . ?
C6 C5 C7 60.08(9) . . ?
C4B C5B H5B 115.2 . . ?
C4B C5B C6B 120.01(10) . . ?
C4B C5B C7B 120.24(12) . . ?
C6B C5B H5B 115.2 . . ?
C7B C5B H5B 115.2 . . ?
C7B C5B C6B 59.80(8) . . ?
C5B C6B H6BA 117.8 . . ?
C5B C6B H6BB 117.8 . . ?
H6BA C6B H6BB 114.9 . . ?
C7B C6B C5B 60.10(8) . . ?
C7B C6B H6BA 117.8 . . ?
C7B C6B H6BB 117.8 . . ?
C5 C7 H7A 117.8 . . ?
C5 C7 H7B 117.8 . . ?
C5 C7 C6 59.85(8) . . ?
H7A C7 H7B 114.9 . . ?
C6 C7 H7A 117.8 . . ?
C6 C7 H7B 117.8 . . ?
C5C C6C H6CA 117.8 . . ?
C5C C6C H6CB 117.8 . . ?
H6CA C6C H6CB 114.9 . . ?
C7C C6C C5C 60.05(8) . . ?
C7C C6C H6CA 117.8 . . ?
C7C C6C H6CB 117.8 . . ?
C5A C6A H6AA 117.8 . . ?
C5A C6A H6AB 117.8 . . ?
C5A C6A C7A 60.07(8) . . ?
H6AA C6A H6AB 114.9 . . ?
C7A C6A H6AA 117.8 . . ?
C7A C6A H6AB 117.8 . . ?
C5 C6 C7 60.07(8) . . ?
C5 C6 H6A 117.8 . . ?
C5 C6 H6B 117.8 . . ?
C7 C6 H6A 117.8 . . ?
C7 C6 H6B 117.8 . . ?
H6A C6 H6B 114.9 . . ?
C5B C7B H7BA 117.8 . . ?
C5B C7B H7BB 117.8 . . ?
C6B C7B C5B 60.09(8) . . ?
C6B C7B H7BA 117.8 . . ?
C6B C7B H7BB 117.8 . . ?
H7BA C7B H7BB 114.9 . . ?
C5C C7C H7CA 117.7 . . ?
C5C C7C H7CB 117.7 . . ?
C6C C7C C5C 60.26(8) . . ?
C6C C7C H7CA 117.7 . . ?
C6C C7C H7CB 117.7 . . ?
H7CA C7C H7CB 114.9 . . ?
C5A C7A C6A 59.85(8) . . ?
C5A C7A H7AA 117.8 . . ?
C5A C7A H7AB 117.8 . . ?
C6A C7A H7AA 117.8 . . ?
C6A C7A H7AB 117.8 . . ?
H7AA C7A H7AB 114.9 . . ?

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
O2B C8B C3B NB 15.95(13) . . . . ?
O2B C8B C3B C4B -106.27(11) . . . . ?
O3C C8C C3C NC -170.99(8) . . . . ?
O3C C8C C3C C4C 67.12(10) . . . . ?
O2A C8A C3A NA -11.37(13) . . . . ?
O2A C8A C3A C4A 110.75(11) . . . . ?
O3B C8B C3B NB -166.58(8) . . . . ?
O3B C8B C3B C4B 71.21(11) . . . . ?
O2C C8C C3C NC 12.02(13) . . . . ?
O2C C8C C3C C4C -109.86(11) . . . . ?
O3A C8A C3A NA 170.45(8) . . . . ?
O3A C8A C3A C4A -67.42(11) . . . . ?
NA C3A C4A C5A 60.27(11) . . . . ?
N C3 C8 O3 175.96(8) . . . . ?
N C3 C8 O2 -4.67(14) . . . . ?
N C3 C4 C5 53.96(11) . . . . ?
NB C3B C4B C5B -63.00(11) . . . . ?
NC C3C C4C C5C -64.44(11) . . . . ?
C1B NB C3B C8B 152.50(9) . . . . ?
C1B NB C3B C4B -87.08(11) . . . . ?
C8A C3A C4A C5A -60.06(11) . . . . ?
C8B C3B C4B C5B 57.26(11) . . . . ?
C1A NA C3A C8A -160.55(9) . . . . ?
C1A NA C3A C4A 78.55(11) . . . . ?
C8C C3C C4C C5C 55.69(11) . . . . ?
C3 N C1 O1 -1.26(14) . . . . ?
C3 N C1 C2 179.03(8) . . . . ?
C3 C4 C5 C7 149.23(10) . . . . ?
C3 C4 C5 C6 78.22(13) . . . . ?
C8 C3 C4 C5 -68.15(11) . . . . ?
C1C NC C3C C8C 159.46(9) . . . . ?
C1C NC C3C C4C -80.83(11) . . . . ?
C1 N C3 C8 -160.91(9) . . . . ?
C1 N C3 C4 75.68(11) . . . . ?
C3C NC C1C O1C 1.65(14) . . . . ?
C3C NC C1C C2C -178.54(9) . . . . ?
C3C C4C C5C C6C -85.99(13) . . . . ?
C3C C4C C5C C7C -156.98(11) . . . . ?
C3A NA C1A O1A 0.37(15) . . . . ?
C3A NA C1A C2A 179.20(9) . . . . ?
C3A C4A C5A C6A 84.96(13) . . . . ?
C3A C4A C5A C7A 155.68(10) . . . . ?
C4 C3 C8 O3 -59.94(11) . . . . ?
C4 C3 C8 O2 119.42(11) . . . . ?
C4 C5 C7 C6 -110.86(13) . . . . ?
C4 C5 C6 C7 108.94(13) . . . . ?
C3B NB C1B O1B 3.04(15) . . . . ?
C3B NB C1B C2B -176.01(9) . . . . ?
C3B C4B C5B C6B -83.77(13) . . . . ?
C3B C4B C5B C7B -154.16(10) . . . . ?
C4C C5C C6C C7C -110.25(14) . . . . ?
C4C C5C C7C C6C 110.09(13) . . . . ?
C4A C5A C6A C7A 109.01(13) . . . . ?
C4A C5A C7A C6A -110.18(13) . . . . ?
C4B C5B C6B C7B -109.68(13) . . . . ?
C4B C5B C7B C6B 109.31(12) . . . . ?

_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
;
