# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_j7-9-3c
_database_code_depnum_ccdc_archive 'CCDC 2022808'
loop_
_audit_author_name
_audit_author_address
'Bing-Xin Zhao'
;Jinan University
China
;
_audit_update_record             
;
2020-08-12 deposited with the CCDC.	2020-09-16 downloaded from the CCDC.
;
_audit_creation_date             2020-08-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H25 N O5, 2(H2 O)'
_chemical_formula_sum            'C18 H29 N O7'
_chemical_formula_weight         371.42
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   6.58016(9)
_cell_length_b                   18.0241(2)
_cell_length_c                   7.96795(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.6953(13)
_cell_angle_gamma                90
_cell_volume                     941.84(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5757
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.4230
_cell_measurement_theta_min      2.4070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6390
_diffrn_reflns_point_group_measured_fraction_full 0.874
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.530
_diffrn_reflns_theta_min         4.907
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -60.00 -19.00   1.00    1.00    --  -41.11 -37.00 -30.00   41
  2  ω    -63.00  24.00   1.00    1.00    --  -41.11  57.00-120.00   87
  3  ω   -111.00 -15.00   1.00    1.00    --  -41.11 -57.00  90.00   96
  4  ω   -113.00 -74.00   1.00    1.00    --  -41.11 -37.00 -30.00   39
  5  ω    -96.00  -3.00   1.00    1.00    --  -41.11 125.00 -90.00   93
  6  ω     75.00 117.00   1.00    1.00    --  106.95  77.00-150.00   42
  7  ω    108.00 169.00   1.00    1.00    --  106.95  77.00-180.00   61
  8  ω    148.00 178.00   1.00    1.00    --  106.95  77.00-150.00   30
  9  ω    124.00 175.00   1.00    1.00    --  106.95  30.00-120.00   51
 10  ω    101.00 175.00   1.00    1.00    --  106.95 125.00  90.00   74
 11  ω     79.00 173.00   1.00    1.00    --  106.95  30.00 150.00   94
 12  ω     57.00 106.00   1.00    1.00    --  106.95 -94.00  90.00   49
 13  ω     40.00 115.00   1.00    1.00    --  106.95 -45.00  90.00   75
 14  ω     34.00 119.00   1.00    1.00    --  106.95-125.00 -30.00   85
 15  ω     61.00 109.00   1.00    1.00    --  106.95 -94.00-180.00   48
 16  ω     34.00  76.00   1.00    1.00    --  106.95 -45.00-150.00   42
 17  ω     24.00  97.00   1.00    1.00    --  106.95 -94.00  30.00   73
 18  ω    -53.00 -18.00   1.00    1.00    --  -41.23 -57.00 150.00   35
 19  ω    -27.00  -2.00   1.00    1.00    --  -41.23 125.00 -30.00   25
 20  ω    -94.00 -68.00   1.00    1.00    --  -41.23 125.00 -30.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1484713000
_diffrn_orient_matrix_UB_12      0.0194642000
_diffrn_orient_matrix_UB_13      0.1530303000
_diffrn_orient_matrix_UB_21      -0.1541624000
_diffrn_orient_matrix_UB_22      -0.0299863000
_diffrn_orient_matrix_UB_23      0.1187876000
_diffrn_orient_matrix_UB_31      0.0967894000
_diffrn_orient_matrix_UB_32      -0.0776936000
_diffrn_orient_matrix_UB_33      -0.0075522000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.665
_reflns_Friedel_fraction_full    0.740
_reflns_Friedel_fraction_max     0.697
_reflns_number_gt                3183
_reflns_number_total             3201
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 
;
 Flack x determined using 1247 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.09(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3201
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0357
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0660P)²+0.1928P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0946
_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:
 O007(H00W,H00X), O008(H00Y,H)
2.b Ternary CH refined with riding coordinates:
 C00H(H00H), C00L(H00L)
2.c Secondary CH2 refined with riding coordinates:
 C00B(H00A,H00B), C00C(H00C,H00D), C00G(H00E,H00F), C00K(H00G,H00I), C00M(H00J,
 H00K), C00N(H00M,H00N), C00O(H00O,H00P)
2.d Aromatic/amide H refined with riding coordinates:
 N006(H006)
2.e Idealised Me refined as rotating group:
 C00P(H00Q,H00R,H00S), C00Q(H00T,H00U,H00V)
2.f Idealised tetrahedral OH refined as rotating group:
 O002(H002), O003(H003)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O001 O 0.1623(2) 0.70447(10) 0.23003(19) 0.0213(4) Uani 1 1 d . . . . .
O002 O 0.5751(3) 0.67102(10) 0.2161(2) 0.0268(4) Uani 1 1 d . . . . .
H002 H 0.4580 0.6867 0.2145 0.040 Uiso 1 1 calc GR . . . .
O003 O 0.3549(3) 0.37615(11) 0.7884(2) 0.0279(4) Uani 1 1 d . . . . .
H003 H 0.2390 0.3634 0.8062 0.042 Uiso 1 1 calc GR . . . .
O004 O 0.2742(3) 0.32032(11) 0.5424(2) 0.0284(4) Uani 1 1 d . . . . .
O005 O 0.7869(3) 0.36062(11) 0.1686(2) 0.0353(5) Uani 1 1 d . . . . .
N006 N 0.0408(3) 0.71492(12) 0.4917(2) 0.0197(4) Uani 1 1 d . . . . .
H006 H -0.0435 0.7506 0.4683 0.024 Uiso 1 1 calc R . . . .
O007 O 0.0114(3) 0.33285(11) 0.8890(2) 0.0330(5) Uani 1 1 d . . . . .
H00W H -0.0408 0.3463 0.9782 0.050 Uiso 1 1 d G . . . .
H00X H -0.0550 0.2962 0.8455 0.050 Uiso 1 1 d G . . . .
O008 O 0.8599(3) 0.62874(15) -0.0117(3) 0.0434(6) Uani 1 1 d . . . . .
H00Y H 0.9602 0.6473 0.0481 0.065 Uiso 1 1 d G . . . .
H H 0.7491 0.6440 0.0240 0.065 Uiso 1 1 d G . . . .
C009 C 0.1547(3) 0.68412(13) 0.3806(3) 0.0166(4) Uani 1 1 d . . . . .
C00A C 0.2752(3) 0.62396(13) 0.4665(3) 0.0152(4) Uani 1 1 d . . . . .
C00B C 0.3280(3) 0.53879(13) 0.2230(3) 0.0163(4) Uani 1 1 d . . . . .
H00A H 0.1975 0.5169 0.2429 0.020 Uiso 1 1 calc R . . . .
H00B H 0.3043 0.5774 0.1389 0.020 Uiso 1 1 calc R . . . .
C00C C 0.5284(3) 0.53941(13) 0.6951(3) 0.0178(5) Uani 1 1 d . . . . .
H00C H 0.5758 0.4993 0.7695 0.021 Uiso 1 1 calc R . . . .
H00D H 0.6382 0.5751 0.6906 0.021 Uiso 1 1 calc R . . . .
C00D C 0.3939(4) 0.35524(13) 0.6359(3) 0.0195(5) Uani 1 1 d . . . . .
C00E C 0.4248(3) 0.57318(13) 0.3881(3) 0.0156(4) Uani 1 1 d . . . . .
C00F C 0.6112(4) 0.35385(14) 0.2043(3) 0.0227(5) Uani 1 1 d . . . . .
C00G C 0.4664(4) 0.47944(13) 0.1573(3) 0.0192(5) Uani 1 1 d . . . . .
H00E H 0.5961 0.5014 0.1352 0.023 Uiso 1 1 calc R . . . .
H00F H 0.4041 0.4594 0.0524 0.023 Uiso 1 1 calc R . . . .
C00H C 0.4687(3) 0.50863(12) 0.5173(3) 0.0144(4) Uani 1 1 d . . . . .
H00H H 0.3350 0.4858 0.5266 0.017 Uiso 1 1 calc R . . . .
C00I C 0.2357(3) 0.62448(13) 0.6293(3) 0.0172(4) Uani 1 1 d . . . . .
C00J C 0.6036(3) 0.44370(13) 0.4596(3) 0.0168(5) Uani 1 1 d . . . . .
C00K C 0.6124(3) 0.62072(14) 0.3537(3) 0.0188(5) Uani 1 1 d . . . . .
H00G H 0.6550 0.6488 0.4544 0.023 Uiso 1 1 calc R . . . .
H00I H 0.7237 0.5880 0.3303 0.023 Uiso 1 1 calc R . . . .
C00L C 0.5018(3) 0.41644(13) 0.2876(3) 0.0176(4) Uani 1 1 d . . . . .
H00L H 0.3668 0.3975 0.3093 0.021 Uiso 1 1 calc R . . . .
C00M C 0.3419(3) 0.57702(13) 0.7630(3) 0.0187(5) Uani 1 1 d . . . . .
H00J H 0.2487 0.5395 0.7984 0.022 Uiso 1 1 calc R . . . .
H00K H 0.3853 0.6073 0.8601 0.022 Uiso 1 1 calc R . . . .
C00N C 0.0752(3) 0.68134(13) 0.6569(3) 0.0190(4) Uani 1 1 d . . . . .
H00M H -0.0479 0.6583 0.6913 0.023 Uiso 1 1 calc R . . . .
H00N H 0.1239 0.7175 0.7408 0.023 Uiso 1 1 calc R . . . .
C00O C 0.6011(3) 0.37871(13) 0.5892(3) 0.0192(4) Uani 1 1 d . . . . .
H00O H 0.6674 0.3361 0.5433 0.023 Uiso 1 1 calc R . . . .
H00P H 0.6818 0.3933 0.6912 0.023 Uiso 1 1 calc R . . . .
C00P C 0.8318(4) 0.46363(14) 0.4550(3) 0.0226(5) Uani 1 1 d . . . . .
H00Q H 0.8524 0.4881 0.3507 0.034 Uiso 1 1 calc GR . . . .
H00R H 0.9121 0.4191 0.4641 0.034 Uiso 1 1 calc GR . . . .
H00S H 0.8725 0.4960 0.5472 0.034 Uiso 1 1 calc GR . . . .
C00Q C 0.4904(5) 0.28557(15) 0.1618(3) 0.0316(6) Uani 1 1 d . . . . .
H00T H 0.5658 0.2537 0.0930 0.047 Uiso 1 1 calc GR . . . .
H00U H 0.3634 0.2989 0.1014 0.047 Uiso 1 1 calc GR . . . .
H00V H 0.4640 0.2601 0.2636 0.047 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O001 C009 1.260(3) . ?
O002 H002 0.8200 . ?
O002 C00K 1.428(3) . ?
O003 H003 0.8200 . ?
O003 C00D 1.317(3) . ?
O004 C00D 1.215(3) . ?
O005 C00F 1.219(3) . ?
N006 H006 0.8600 . ?
N006 C009 1.327(3) . ?
N006 C00N 1.450(3) . ?
O007 H00W 0.8498 . ?
O007 H00X 0.8500 . ?
O008 H00Y 0.8500 . ?
O008 H 0.8500 . ?
C009 C00A 1.478(3) . ?
C00A C00E 1.515(3) . ?
C00A C00I 1.344(3) . ?
C00B H00A 0.9700 . ?
C00B H00B 0.9700 . ?
C00B C00E 1.544(3) . ?
C00B C00G 1.525(3) . ?
C00C H00C 0.9700 . ?
C00C H00D 0.9700 . ?
C00C C00H 1.542(3) . ?
C00C C00M 1.539(3) . ?
C00D C00O 1.503(3) . ?
C00E C00H 1.564(3) . ?
C00E C00K 1.546(3) . ?
C00F C00L 1.520(3) . ?
C00F C00Q 1.489(4) . ?
C00G H00E 0.9700 . ?
C00G H00F 0.9700 . ?
C00G C00L 1.544(3) . ?
C00H H00H 0.9800 . ?
C00H C00J 1.561(3) . ?
C00I C00M 1.494(3) . ?
C00I C00N 1.501(3) . ?
C00J C00L 1.555(3) . ?
C00J C00O 1.563(3) . ?
C00J C00P 1.547(3) . ?
C00K H00G 0.9700 . ?
C00K H00I 0.9700 . ?
C00L H00L 0.9800 . ?
C00M H00J 0.9700 . ?
C00M H00K 0.9700 . ?
C00N H00M 0.9700 . ?
C00N H00N 0.9700 . ?
C00O H00O 0.9700 . ?
C00O H00P 0.9700 . ?
C00P H00Q 0.9600 . ?
C00P H00R 0.9600 . ?
C00P H00S 0.9600 . ?
C00Q H00T 0.9600 . ?
C00Q H00U 0.9600 . ?
C00Q H00V 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C00K O002 H002 109.5 . . ?
C00D O003 H003 109.5 . . ?
C009 N006 H006 124.0 . . ?
C009 N006 C00N 112.08(19) . . ?
C00N N006 H006 124.0 . . ?
H00W O007 H00X 109.5 . . ?
H00Y O008 H 109.5 . . ?
O001 C009 N006 125.6(2) . . ?
O001 C009 C00A 126.4(2) . . ?
N006 C009 C00A 108.01(18) . . ?
C009 C00A C00E 126.47(18) . . ?
C00I C00A C009 107.63(19) . . ?
C00I C00A C00E 125.8(2) . . ?
H00A C00B H00B 108.0 . . ?
C00E C00B H00A 109.4 . . ?
C00E C00B H00B 109.4 . . ?
C00G C00B H00A 109.4 . . ?
C00G C00B H00B 109.4 . . ?
C00G C00B C00E 111.00(17) . . ?
H00C C00C H00D 108.3 . . ?
C00H C00C H00C 109.8 . . ?
C00H C00C H00D 109.8 . . ?
C00M C00C H00C 109.8 . . ?
C00M C00C H00D 109.8 . . ?
C00M C00C C00H 109.34(17) . . ?
O003 C00D C00O 113.36(19) . . ?
O004 C00D O003 123.3(2) . . ?
O004 C00D C00O 123.4(2) . . ?
C00A C00E C00B 110.93(17) . . ?
C00A C00E C00H 105.63(17) . . ?
C00A C00E C00K 107.06(18) . . ?
C00B C00E C00H 107.64(18) . . ?
C00B C00E C00K 110.55(17) . . ?
C00K C00E C00H 114.95(17) . . ?
O005 C00F C00L 121.3(2) . . ?
O005 C00F C00Q 121.9(2) . . ?
C00Q C00F C00L 116.7(2) . . ?
C00B C00G H00E 109.6 . . ?
C00B C00G H00F 109.6 . . ?
C00B C00G C00L 110.26(17) . . ?
H00E C00G H00F 108.1 . . ?
C00L C00G H00E 109.6 . . ?
C00L C00G H00F 109.6 . . ?
C00C C00H C00E 110.86(18) . . ?
C00C C00H H00H 104.1 . . ?
C00C C00H C00J 115.59(17) . . ?
C00E C00H H00H 104.1 . . ?
C00J C00H C00E 116.30(17) . . ?
C00J C00H H00H 104.1 . . ?
C00A C00I C00M 124.6(2) . . ?
C00A C00I C00N 109.9(2) . . ?
C00M C00I C00N 125.47(19) . . ?
C00H C00J C00O 109.30(17) . . ?
C00L C00J C00H 106.37(16) . . ?
C00L C00J C00O 108.58(18) . . ?
C00P C00J C00H 114.17(18) . . ?
C00P C00J C00L 113.66(18) . . ?
C00P C00J C00O 104.64(17) . . ?
O002 C00K C00E 113.49(18) . . ?
O002 C00K H00G 108.9 . . ?
O002 C00K H00I 108.9 . . ?
C00E C00K H00G 108.9 . . ?
C00E C00K H00I 108.9 . . ?
H00G C00K H00I 107.7 . . ?
C00F C00L C00G 107.62(17) . . ?
C00F C00L C00J 115.74(18) . . ?
C00F C00L H00L 106.6 . . ?
C00G C00L C00J 113.02(19) . . ?
C00G C00L H00L 106.6 . . ?
C00J C00L H00L 106.6 . . ?
C00C C00M H00J 109.7 . . ?
C00C C00M H00K 109.7 . . ?
C00I C00M C00C 109.96(18) . . ?
C00I C00M H00J 109.7 . . ?
C00I C00M H00K 109.7 . . ?
H00J C00M H00K 108.2 . . ?
N006 C00N C00I 102.23(18) . . ?
N006 C00N H00M 111.3 . . ?
N006 C00N H00N 111.3 . . ?
C00I C00N H00M 111.3 . . ?
C00I C00N H00N 111.3 . . ?
H00M C00N H00N 109.2 . . ?
C00D C00O C00J 115.67(18) . . ?
C00D C00O H00O 108.4 . . ?
C00D C00O H00P 108.4 . . ?
C00J C00O H00O 108.4 . . ?
C00J C00O H00P 108.4 . . ?
H00O C00O H00P 107.4 . . ?
C00J C00P H00Q 109.5 . . ?
C00J C00P H00R 109.5 . . ?
C00J C00P H00S 109.5 . . ?
H00Q C00P H00R 109.5 . . ?
H00Q C00P H00S 109.5 . . ?
H00R C00P H00S 109.5 . . ?
C00F C00Q H00T 109.5 . . ?
C00F C00Q H00U 109.5 . . ?
C00F C00Q H00V 109.5 . . ?
H00T C00Q H00U 109.5 . . ?
H00T C00Q H00V 109.5 . . ?
H00U C00Q H00V 109.5 . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.920
_oxdiff_exptl_absorpt_empirical_full_min 0.518
####################################################################### 
# 
# 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_c11f
_database_code_depnum_ccdc_archive 'CCDC 2022811'
loop_
_audit_author_name
_audit_author_address
'Bing-Xin Zhao'
;Jinan University
China
;
_audit_update_record             
;
2020-08-12 deposited with the CCDC.	2020-09-16 downloaded from the CCDC.
;
_audit_creation_date             2020-08-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C19 H22 O6'
_chemical_formula_sum            'C19 H22 O6'
_chemical_formula_weight         346.36
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   10.1810(2)
_cell_length_b                   12.4105(2)
_cell_length_c                   12.7012(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1604.81(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5155
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.0390
_cell_measurement_theta_min      3.4570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.076
_diffrn_reflns_theta_min         4.982
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -121.00   0.00   1.00    1.00    --  -40.98 -19.00  60.00  121
  2  ω     23.00  97.00   1.00    1.00    --   40.98-125.00 -60.00   74
  3  ω      1.00  82.00   1.00    1.00    --   40.98 -99.00 -60.00   81
  4  ω     94.00 178.00   1.00    1.00    --  106.95 125.00 -60.00   84
  5  ω     34.00 121.00   1.00    1.00    --  106.95-125.00-180.00   87
  6  ω     78.00 178.00   1.00    1.00    --  106.95  61.00   0.00  100
  7  ω     31.00 135.00   1.00    1.00    --  106.95 -30.00  30.00  104
  8  ω     78.00 178.00   1.00    1.00    --  106.95  61.00  90.00  100
  9  ω    100.00 178.00   1.00    1.00    --  106.95 111.00-156.00   78
 10  ω     94.00 108.00   1.00    1.00    --  106.95 125.00  30.00   14
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0214421000
_diffrn_orient_matrix_UB_12      0.1109814000
_diffrn_orient_matrix_UB_13      0.0515799000
_diffrn_orient_matrix_UB_21      0.0295311000
_diffrn_orient_matrix_UB_22      -0.0491746000
_diffrn_orient_matrix_UB_23      0.1087836000
_diffrn_orient_matrix_UB_31      0.1468530000
_diffrn_orient_matrix_UB_32      0.0261448000
_diffrn_orient_matrix_UB_33      -0.0144216000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.717
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                3092
_reflns_number_total             3142
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 
;
 Flack x determined using 1257 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3142
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0513
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0863P)²+1.1964P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1447
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C14(H14), C23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C17(H17A,H17B), C19(H19A,H19B), C21(H21A,
 H21B), C22(H22A,H22B)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.1084(3) -0.2771(2) -0.5790(2) 0.0248(6) Uani 1 1 d . . . . .
H1 H -0.1573 -0.2328 -0.6065 0.037 Uiso 1 1 calc GR . . . .
O2 O -0.1987(2) -1.07588(19) -0.6509(2) 0.0215(5) Uani 1 1 d . . . . .
O3 O -0.0072(2) -0.63999(19) -0.61243(19) 0.0182(5) Uani 1 1 d . . . . .
O4 O -0.0850(3) -0.9873(2) -0.5264(2) 0.0243(6) Uani 1 1 d . . . . .
C5 C -0.1498(3) -0.3784(3) -0.6033(3) 0.0204(7) Uani 1 1 d . . . . .
O6 O -0.3945(3) -1.0926(2) -0.7457(3) 0.0346(7) Uani 1 1 d . . . . .
H6 H -0.3878 -1.1579 -0.7538 0.052 Uiso 1 1 calc GR . . . .
O7 O -0.3179(3) -0.3062(2) -0.7063(3) 0.0362(7) Uani 1 1 d . . . . .
C8 C -0.2045(3) -0.8903(3) -0.6622(3) 0.0184(7) Uani 1 1 d . . . . .
C9 C -0.2106(3) -0.5835(3) -0.6973(3) 0.0177(7) Uani 1 1 d . . . . .
C10 C -0.1256(3) -0.5781(3) -0.5969(3) 0.0170(7) Uani 1 1 d . . . . .
C11 C -0.1994(4) -0.6278(3) -0.5021(3) 0.0212(7) Uani 1 1 d . . . . .
H11A H -0.2856 -0.5952 -0.4956 0.025 Uiso 1 1 calc R . . . .
H11B H -0.1510 -0.6139 -0.4377 0.025 Uiso 1 1 calc R . . . .
C12 C -0.0808(3) -0.4652(3) -0.5708(3) 0.0193(7) Uani 1 1 d . . . . .
C13 C -0.2134(4) -0.7507(3) -0.5192(3) 0.0207(7) Uani 1 1 d . . . . .
H13A H -0.1537 -0.7894 -0.4733 0.025 Uiso 1 1 calc R . . . .
H13B H -0.3024 -0.7735 -0.5034 0.025 Uiso 1 1 calc R . . . .
C14 C -0.2671(3) -0.7003(3) -0.7049(3) 0.0167(7) Uani 1 1 d . . . . .
H14 H -0.3550 -0.6988 -0.6733 0.020 Uiso 1 1 calc R . . . .
C15 C -0.1807(3) -0.7747(3) -0.6350(3) 0.0173(7) Uani 1 1 d . . . . .
C16 C -0.1539(3) -0.9837(3) -0.6030(3) 0.0198(7) Uani 1 1 d . . . . .
C17 C -0.3202(3) -0.4987(3) -0.6903(3) 0.0211(7) Uani 1 1 d . . . . .
H17A H -0.3694 -0.4984 -0.7556 0.025 Uiso 1 1 calc R . . . .
H17B H -0.3801 -0.5182 -0.6340 0.025 Uiso 1 1 calc R . . . .
C18 C -0.2669(4) -0.3876(3) -0.6700(3) 0.0236(8) Uani 1 1 d . . . . .
C19 C -0.3452(4) -0.8553(3) -0.8196(3) 0.0225(8) Uani 1 1 d . . . . .
H19A H -0.4374 -0.8501 -0.8010 0.027 Uiso 1 1 calc R . . . .
H19B H -0.3388 -0.8858 -0.8897 0.027 Uiso 1 1 calc R . . . .
C20 C -0.2757(3) -0.9260(3) -0.7429(3) 0.0197(7) Uani 1 1 d . . . . .
C21 C -0.2828(4) -0.7432(3) -0.8180(3) 0.0205(7) Uani 1 1 d . . . . .
H21A H -0.3371 -0.6939 -0.8581 0.025 Uiso 1 1 calc R . . . .
H21B H -0.1972 -0.7464 -0.8515 0.025 Uiso 1 1 calc R . . . .
C22 C -0.0350(3) -0.7477(3) -0.6501(3) 0.0181(7) Uani 1 1 d . . . . .
H22A H 0.0183 -0.7993 -0.6118 0.022 Uiso 1 1 calc R . . . .
H22B H -0.0126 -0.7529 -0.7241 0.022 Uiso 1 1 calc R . . . .
C23 C -0.2733(4) -1.0475(3) -0.7455(3) 0.0241(8) Uani 1 1 d . . . . .
H23 H -0.2249 -1.0715 -0.8079 0.029 Uiso 1 1 calc R . . . .
C24 C -0.1255(4) -0.5539(3) -0.7948(3) 0.0207(7) Uani 1 1 d . . . . .
H24A H -0.0875 -0.4839 -0.7848 0.031 Uiso 1 1 calc GR . . . .
H24B H -0.1797 -0.5533 -0.8567 0.031 Uiso 1 1 calc GR . . . .
H24C H -0.0569 -0.6062 -0.8032 0.031 Uiso 1 1 calc GR . . . .
C25 C 0.0404(4) -0.4521(3) -0.5052(3) 0.0255(8) Uani 1 1 d . . . . .
H25A H 0.1166 -0.4660 -0.5477 0.038 Uiso 1 1 calc GR . . . .
H25B H 0.0380 -0.5020 -0.4475 0.038 Uiso 1 1 calc GR . . . .
H25C H 0.0444 -0.3798 -0.4785 0.038 Uiso 1 1 calc GR . . . .


_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 C5 1.362(4) . ?
O2 C16 1.374(4) . ?
O2 C23 1.464(4) . ?
O3 C10 1.444(4) . ?
O3 C22 1.448(4) . ?
O4 C16 1.201(5) . ?
C5 C12 1.352(5) . ?
C5 C18 1.466(5) . ?
O6 C23 1.355(5) . ?
O7 C18 1.226(5) . ?
C8 C15 1.495(5) . ?
C8 C16 1.474(5) . ?
C8 C20 1.331(5) . ?
C9 C10 1.542(5) . ?
C9 C14 1.562(4) . ?
C9 C17 1.536(5) . ?
C9 C24 1.556(5) . ?
C10 C11 1.547(5) . ?
C10 C12 1.510(5) . ?
C11 C13 1.548(5) . ?
C12 C25 1.498(5) . ?
C13 C15 1.537(5) . ?
C14 C15 1.554(5) . ?
C14 C21 1.540(5) . ?
C15 C22 1.532(5) . ?
C17 C18 1.505(5) . ?
C19 C20 1.490(5) . ?
C19 C21 1.529(5) . ?
C20 C23 1.507(5) . ?

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
C16 O2 C23 109.6(2) . . ?
C10 O3 C22 111.9(2) . . ?
O1 C5 C18 117.1(3) . . ?
C12 C5 O1 120.4(3) . . ?
C12 C5 C18 122.5(3) . . ?
C16 C8 C15 125.4(3) . . ?
C20 C8 C15 125.9(3) . . ?
C20 C8 C16 108.7(3) . . ?
C10 C9 C14 107.4(3) . . ?
C10 C9 C24 109.6(3) . . ?
C17 C9 C10 109.3(3) . . ?
C17 C9 C14 111.8(3) . . ?
C17 C9 C24 106.8(3) . . ?
C24 C9 C14 112.0(3) . . ?
O3 C10 C9 109.4(3) . . ?
O3 C10 C11 107.4(3) . . ?
O3 C10 C12 105.7(3) . . ?
C9 C10 C11 110.7(3) . . ?
C12 C10 C9 113.1(3) . . ?
C12 C10 C11 110.2(3) . . ?
C10 C11 C13 109.2(3) . . ?
C5 C12 C10 121.0(3) . . ?
C5 C12 C25 120.8(3) . . ?
C25 C12 C10 118.2(3) . . ?
C15 C13 C11 107.8(3) . . ?
C15 C14 C9 107.9(3) . . ?
C21 C14 C9 114.6(3) . . ?
C21 C14 C15 112.7(3) . . ?
C8 C15 C13 111.8(3) . . ?
C8 C15 C14 110.3(3) . . ?
C8 C15 C22 109.7(3) . . ?
C13 C15 C14 108.0(3) . . ?
C22 C15 C13 106.7(3) . . ?
C22 C15 C14 110.3(3) . . ?
O2 C16 C8 108.2(3) . . ?
O4 C16 O2 121.4(3) . . ?
O4 C16 C8 130.3(3) . . ?
C18 C17 C9 112.1(3) . . ?
C5 C18 C17 117.6(3) . . ?
O7 C18 C5 119.8(3) . . ?
O7 C18 C17 122.5(3) . . ?
C20 C19 C21 109.3(3) . . ?
C8 C20 C19 124.4(3) . . ?
C8 C20 C23 110.0(3) . . ?
C19 C20 C23 125.6(3) . . ?
C19 C21 C14 111.7(3) . . ?
O3 C22 C15 110.5(3) . . ?
O2 C23 C20 103.4(3) . . ?
O6 C23 O2 112.0(3) . . ?
O6 C23 C20 113.5(3) . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.470
_oxdiff_exptl_absorpt_empirical_full_min 0.670
####################################################################### 
# 
# 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_c11e
_database_code_depnum_ccdc_archive 'CCDC 2022810'
loop_
_audit_author_name
_audit_author_address
'Bing-Xin Zhao'
;Jinan University
China
;
_audit_update_record             
;
2020-08-12 deposited with the CCDC.	2020-09-16 downloaded from the CCDC.
;
_audit_creation_date             2020-08-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C19 H22 O6'
_chemical_formula_sum            'C19 H22 O6'
_chemical_formula_weight         346.36
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   9.28120(10)
_cell_length_b                   11.92810(10)
_cell_length_c                   14.17700(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1569.49(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14657
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.5050
_cell_measurement_theta_min      3.0730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19454
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.711
_diffrn_reflns_theta_min         4.845
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00 -13.00   1.00    1.00    --  -40.98 -57.00 -30.00  100
  2  ω   -113.00 -65.00   1.00    1.00    --  -40.98-138.00  93.00   48
  3  ω    -33.00  65.00   1.00    1.00    --   40.98 -37.00 -60.00   98
  4  ω     31.00 135.00   1.00    1.00    --  106.95 -30.00 -90.00  104
  5  ω     94.00 178.00   1.00    1.00    --  106.95 125.00  90.00   84
  6  ω     79.00 178.00   1.00    1.00    --  106.95  30.00 -90.00   99
  7  ω     81.00 178.00   1.00    1.00    --  106.95  45.00  30.00   97
  8  ω     35.00 136.00   1.00    1.00    --  106.95 -61.00-180.00  101
  9  ω     24.00 109.00   1.00    1.00    --  106.95 -94.00  30.00   85
 10  ω   -113.00 -13.00   1.00    1.00    --  -40.98 -57.00  90.00  100
 11  ω   -113.00 -13.00   1.00    1.00    --  -40.98 -57.00-150.00  100
 12  ω     74.00 178.00   1.00    1.00    --  106.95  77.00 -60.00  104
 13  ω     24.00 109.00   1.00    1.00    --  106.95 -94.00 120.00   85
 14  ω     81.00 178.00   1.00    1.00    --  106.95  45.00-150.00   97
 15  ω     54.00 178.00   1.00    1.00    --  106.95  15.00 150.00  124
 16  ω      1.00  82.00   1.00    1.00    --   40.98 -99.00  90.00   81
 17  ω      1.00  82.00   1.00    1.00    --   40.98 -99.00-150.00   81
 18  ω     81.00 178.00   1.00    1.00    --  106.95  45.00   0.00   97
 19  ω     81.00 178.00   1.00    1.00    --  106.95  45.00  60.00   97
 20  ω     78.00 178.00   1.00    1.00    --  106.95  61.00 -90.00  100
 21  ω     74.00 178.00   1.00    1.00    --  106.95  77.00 150.00  104
 22  ω   -117.00 -38.00   1.00    1.00    --  -40.98 -77.00 -60.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0380537000
_diffrn_orient_matrix_UB_12      -0.1024780000
_diffrn_orient_matrix_UB_13      0.0612493000
_diffrn_orient_matrix_UB_21      0.0214152000
_diffrn_orient_matrix_UB_22      -0.0708571000
_diffrn_orient_matrix_UB_23      -0.0897157000
_diffrn_orient_matrix_UB_31      0.1602686000
_diffrn_orient_matrix_UB_32      0.0337033000
_diffrn_orient_matrix_UB_33      -0.0025452000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.726
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                3109
_reflns_number_total             3134
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 
;
 Flack x determined using 1298 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3134
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0326
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0571P)²+0.3975P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0861
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C013(H013), C022(H022)
2.b Secondary CH2 refined with riding coordinates:
 C007(H00A,H00B), C018(H01D,H01E), C019(H01F,H01G), C021(H02D,H02E), C023(H02F,
 H02G), C024(H02H,H02I)
2.c Idealised Me refined as rotating group:
 C015(H01A,H01B,H01C), C020(H02A,H02B,H02C)
2.d Idealised tetrahedral OH refined as rotating group:
 O005(H005), O006(H006)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O001 O -0.56656(15) -0.10534(11) -0.04937(9) 0.0153(3) Uani 1 1 d . . . . .
O002 O -0.12629(16) -0.07579(14) -0.29366(11) 0.0244(3) Uani 1 1 d . . . . .
O003 O -1.06786(16) 0.18797(12) -0.10973(10) 0.0206(3) Uani 1 1 d . . . . .
O004 O -1.11916(16) 0.23038(12) -0.26014(10) 0.0216(3) Uani 1 1 d . . . . .
O005 O -0.07161(15) -0.13573(12) -0.11506(10) 0.0191(3) Uani 1 1 d . . . . .
H005 H -0.0281 -0.1545 -0.1629 0.029 Uiso 1 1 calc GR . . . .
O006 O -0.99916(17) 0.05344(14) 0.00093(10) 0.0233(3) Uani 1 1 d . . . . .
H006 H -1.0197 -0.0026 -0.0297 0.035 Uiso 1 1 calc GR . . . .
C007 C -0.7095(2) -0.06793(16) -0.07325(13) 0.0145(4) Uani 1 1 d . . . . .
H00A H -0.7674 -0.0626 -0.0165 0.017 Uiso 1 1 calc R . . . .
H00B H -0.7546 -0.1219 -0.1151 0.017 Uiso 1 1 calc R . . . .
C008 C -0.2243(2) -0.06022(16) -0.23735(14) 0.0168(4) Uani 1 1 d . . . . .
C009 C -0.2072(2) -0.09846(15) -0.13912(13) 0.0153(4) Uani 1 1 d . . . . .
C010 C -0.4923(2) -0.04442(16) -0.20538(13) 0.0129(4) Uani 1 1 d . . . . .
C011 C -0.3143(2) -0.09919(16) -0.07546(13) 0.0148(4) Uani 1 1 d . . . . .
C012 C -0.4561(2) -0.04393(15) -0.09871(13) 0.0137(4) Uani 1 1 d . . . . .
C013 C -0.6249(2) 0.03471(15) -0.21821(12) 0.0124(4) Uani 1 1 d . . . . .
H013 H -0.5860 0.1089 -0.2335 0.015 Uiso 1 1 calc R . . . .
C014 C -1.0396(2) 0.18614(17) -0.20422(14) 0.0168(4) Uani 1 1 d . . . . .
C015 C -0.5221(2) -0.16528(15) -0.23841(14) 0.0170(4) Uani 1 1 d . . . . .
H01A H -0.4403 -0.2116 -0.2243 0.026 Uiso 1 1 calc GR . . . .
H01B H -0.5391 -0.1656 -0.3052 0.026 Uiso 1 1 calc GR . . . .
H01C H -0.6054 -0.1939 -0.2063 0.026 Uiso 1 1 calc GR . . . .
C016 C -0.9035(2) 0.12515(15) -0.22015(13) 0.0149(4) Uani 1 1 d . . . . .
C017 C -0.8481(2) 0.09809(16) -0.13627(13) 0.0149(4) Uani 1 1 d . . . . .
C018 C -0.6099(2) 0.12245(16) -0.05773(13) 0.0163(4) Uani 1 1 d . . . . .
H01D H -0.6113 0.1989 -0.0809 0.020 Uiso 1 1 calc R . . . .
H01E H -0.6477 0.1221 0.0061 0.020 Uiso 1 1 calc R . . . .
C019 C -0.8399(2) 0.09591(17) -0.31356(13) 0.0172(4) Uani 1 1 d . . . . .
H01F H -0.7952 0.1615 -0.3414 0.021 Uiso 1 1 calc R . . . .
H01G H -0.9147 0.0696 -0.3559 0.021 Uiso 1 1 calc R . . . .
C020 C -0.2958(2) -0.14689(18) 0.02144(14) 0.0206(4) Uani 1 1 d . . . . .
H02A H -0.2004 -0.1770 0.0277 0.031 Uiso 1 1 calc GR . . . .
H02B H -0.3652 -0.2054 0.0313 0.031 Uiso 1 1 calc GR . . . .
H02C H -0.3100 -0.0888 0.0674 0.031 Uiso 1 1 calc GR . . . .
C021 C -0.7272(2) 0.00377(16) -0.29858(13) 0.0151(4) Uani 1 1 d . . . . .
H02D H -0.7752 -0.0663 -0.2839 0.018 Uiso 1 1 calc R . . . .
H02E H -0.6725 -0.0067 -0.3562 0.018 Uiso 1 1 calc R . . . .
C022 C -0.9484(2) 0.13592(18) -0.05904(14) 0.0186(4) Uani 1 1 d . . . . .
H022 H -0.8997 0.1935 -0.0214 0.022 Uiso 1 1 calc R . . . .
C023 C -0.4546(2) 0.07663(16) -0.05850(14) 0.0171(4) Uani 1 1 d . . . . .
H02F H -0.4160 0.0762 0.0051 0.021 Uiso 1 1 calc R . . . .
H02G H -0.3938 0.1242 -0.0972 0.021 Uiso 1 1 calc R . . . .
C024 C -0.3627(2) -0.00122(16) -0.26196(13) 0.0163(4) Uani 1 1 d . . . . .
H02H H -0.3818 -0.0111 -0.3287 0.020 Uiso 1 1 calc R . . . .
H02I H -0.3513 0.0784 -0.2503 0.020 Uiso 1 1 calc R . . . .
C1 C -0.7027(2) 0.04683(15) -0.12169(13) 0.0134(4) Uani 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
O001 C007 1.440(2) . ?
O001 C012 1.441(2) . ?
O002 C008 1.224(3) . ?
O003 C014 1.365(2) . ?
O003 C022 1.460(2) . ?
O004 C014 1.205(3) . ?
O005 C009 1.377(2) . ?
O006 C022 1.383(3) . ?
C007 C1 1.533(2) . ?
C008 C009 1.474(3) . ?
C008 C024 1.506(3) . ?
C009 C011 1.343(3) . ?
C010 C012 1.549(2) . ?
C010 C013 1.562(3) . ?
C010 C015 1.541(3) . ?
C010 C024 1.535(3) . ?
C011 C012 1.508(3) . ?
C011 C020 1.497(3) . ?
C012 C023 1.547(2) . ?
C013 C021 1.528(2) . ?
C013 C1 1.554(2) . ?
C014 C016 1.475(3) . ?
C016 C017 1.335(3) . ?
C016 C019 1.491(3) . ?
C017 C022 1.507(3) . ?
C017 C1 1.496(3) . ?
C018 C023 1.541(3) . ?
C018 C1 1.542(3) . ?
C019 C021 1.532(3) . ?

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
C007 O001 C012 112.57(13) . . ?
C014 O003 C022 109.29(15) . . ?
O001 C007 C1 110.15(15) . . ?
O002 C008 C009 119.29(19) . . ?
O002 C008 C024 123.60(18) . . ?
C009 C008 C024 117.09(17) . . ?
O005 C009 C008 115.60(17) . . ?
C011 C009 O005 120.53(17) . . ?
C011 C009 C008 123.86(18) . . ?
C012 C010 C013 106.40(14) . . ?
C015 C010 C012 109.83(15) . . ?
C015 C010 C013 112.86(15) . . ?
C024 C010 C012 109.82(15) . . ?
C024 C010 C013 110.72(15) . . ?
C024 C010 C015 107.22(15) . . ?
C009 C011 C012 119.76(17) . . ?
C009 C011 C020 122.30(18) . . ?
C020 C011 C012 117.82(17) . . ?
O001 C012 C010 108.52(15) . . ?
O001 C012 C011 107.00(14) . . ?
O001 C012 C023 107.45(15) . . ?
C011 C012 C010 113.63(16) . . ?
C011 C012 C023 108.56(15) . . ?
C023 C012 C010 111.42(15) . . ?
C021 C013 C010 115.51(15) . . ?
C021 C013 C1 112.96(15) . . ?
C1 C013 C010 108.66(14) . . ?
O003 C014 C016 108.83(16) . . ?
O004 C014 O003 121.38(18) . . ?
O004 C014 C016 129.79(18) . . ?
C014 C016 C019 126.17(17) . . ?
C017 C016 C014 108.23(17) . . ?
C017 C016 C019 125.59(18) . . ?
C016 C017 C022 109.67(17) . . ?
C016 C017 C1 124.71(18) . . ?
C1 C017 C022 125.43(17) . . ?
C023 C018 C1 108.10(15) . . ?
C016 C019 C021 108.35(15) . . ?
C013 C021 C019 110.76(15) . . ?
O003 C022 C017 103.83(15) . . ?
O006 C022 O003 110.28(16) . . ?
O006 C022 C017 116.37(17) . . ?
C018 C023 C012 108.91(15) . . ?
C008 C024 C010 112.98(15) . . ?
C007 C1 C013 109.30(14) . . ?
C007 C1 C018 106.36(15) . . ?
C017 C1 C007 112.96(15) . . ?
C017 C1 C013 109.62(15) . . ?
C017 C1 C018 110.24(15) . . ?
C018 C1 C013 108.22(15) . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.550
_oxdiff_exptl_absorpt_empirical_full_min 0.528
####################################################################### 
# 
# 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_j8-7-5-5d
_database_code_depnum_ccdc_archive 'CCDC 2022809'
loop_
_audit_author_name
_audit_author_address
'Bing-Xin Zhao'
;Jinan University
China
;
_audit_update_record             
;
2020-08-12 deposited with the CCDC.	2020-09-16 downloaded from the CCDC.
;
_audit_creation_date             2020-08-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C19 H24 N O5.5, H2 O'
_chemical_formula_sum            'C19 H27 N O7'
_chemical_formula_weight         381.41
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.91520(10)
_cell_length_b                   18.3839(2)
_cell_length_c                   7.54850(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1792.25(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17480
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.3800
_cell_measurement_theta_min      2.3570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            20012
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.640
_diffrn_reflns_theta_min         4.183
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -117.00  -9.00   1.00    1.00    --  -41.11 -77.00  30.00  108
  2  ω     17.00 115.00   1.00    1.00    --   41.11  38.00  90.00   98
  3  ω      1.00  82.00   1.00    1.00    --   41.11 -99.00  60.00   81
  4  ω     25.00 109.00   1.00    1.00    --  106.95 -95.00 -30.00   84
  5  ω     81.00 178.00   1.00    1.00    --  106.95  45.00-120.00   97
  6  ω     94.00 178.00   1.00    1.00    --  106.95 125.00 -60.00   84
  7  ω     25.00 160.00   1.00    1.00    --  106.95 -15.00-150.00  135
  8  ω     94.00 178.00   1.00    1.00    --  106.95 125.00 150.00   84
  9  ω     34.00 133.00   1.00    1.00    --  106.95 -45.00 -60.00   99
 10  ω      9.00 117.00   1.00    1.00    --   41.11  77.00-180.00  108
 11  ω      9.00 117.00   1.00    1.00    --   41.11  77.00 -60.00  108
 12  ω     74.00 178.00   1.00    1.00    --  106.95  77.00   0.00  104
 13  ω     74.00 178.00   1.00    1.00    --  106.95  77.00  60.00  104
 14  ω     34.00 121.00   1.00    1.00    --  106.95-125.00 150.00   87
 15  ω     81.00 178.00   1.00    1.00    --  106.95  45.00 -60.00   97
 16  ω      1.00  82.00   1.00    1.00    --   41.11 -99.00 -90.00   81
 17  ω     13.00 113.00   1.00    1.00    --   41.11  57.00 150.00  100
 18  ω     78.00 178.00   1.00    1.00    --  106.95  61.00 120.00  100
 19  ω     78.00 135.00   1.00    1.00    --  106.95  61.00-180.00   57
 20  ω     34.00 121.00   1.00    1.00    --  106.95-125.00 -60.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0750370000
_diffrn_orient_matrix_UB_12      -0.0211596000
_diffrn_orient_matrix_UB_13      0.0765106000
_diffrn_orient_matrix_UB_21      0.0439178000
_diffrn_orient_matrix_UB_22      0.1120096000
_diffrn_orient_matrix_UB_23      0.0224972000
_diffrn_orient_matrix_UB_31      -0.1846601000
_diffrn_orient_matrix_UB_32      0.0351418000
_diffrn_orient_matrix_UB_33      -0.0257120000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                3580
_reflns_number_total             3604
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 
;
 Flack x determined using 1477 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3604
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0397
_refine_ls_restrained_S_all      1.146
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0478P)²+1.1012P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1066
_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. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(O1A)
3. Others
 Sof(O1A)=Sof(H1AA)=Sof(H1AB)=1-FVAR(1)
 Sof(O1)=Sof(H1A)=Sof(H1B)=FVAR(1)
 Fixed Sof: H00U(0.5) H00V(0.5)
4.a Free rotating group:
 O004(H00U,H00V), O1(H1A,H1B), O1A(H1AA,H1AB)
4.b Ternary CH refined with riding coordinates:
 C00E(H00F), C00I(H00I)
4.c Secondary CH2 refined with riding coordinates:
 C009(H00A,H00B), C00F(H00G,H00H), C00J(H00J,H00K), C00L(H00L,H00M), C00O(H00Q,
 H00R), C00Q(H00S,H00T)
4.d Aromatic/amide H refined with riding coordinates:
 N007(H007)
4.e Idealised Me refined as rotating group:
 C00D(H00C,H00D,H00E), C00N(H00N,H00O,H00P)
4.f Idealised tetrahedral OH refined as rotating group:
 O001(H001), O005(H005)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O001 O 0.81068(15) 0.44129(11) 0.9628(2) 0.0216(4) Uani 1 1 d . . . . .
H001 H 0.8683 0.4600 0.9588 0.032 Uiso 1 1 calc GR . . . .
O002 O 0.76008(15) 0.29986(10) 0.7855(3) 0.0199(4) Uani 1 1 d . . . . .
O003 O 0.26306(14) 0.40172(11) 0.4414(3) 0.0227(4) Uani 1 1 d . . . . .
O004 O 1.0000 0.5000 1.0323(4) 0.0262(6) Uani 1 2 d S T P . .
H00U H 0.9819 0.5343 1.1011 0.039 Uiso 0.5 1 d G . . . .
H00V H 1.0610 0.5079 0.9946 0.039 Uiso 0.5 1 d G . . . .
O005 O 1.09867(14) 0.36355(12) 0.6392(3) 0.0248(5) Uani 1 1 d . . . . .
H005 H 1.1308 0.3789 0.5533 0.037 Uiso 1 1 calc GR . . . .
O006 O 1.03350(15) 0.41446(13) 0.3285(3) 0.0273(5) Uani 1 1 d . . . . .
N007 N 0.32641(17) 0.38286(12) 0.7232(3) 0.0198(5) Uani 1 1 d . . . . .
H007 H 0.2683 0.3848 0.7787 0.024 Uiso 1 1 calc R . . . .
C008 C 0.3359(2) 0.39084(14) 0.5468(4) 0.0191(5) Uani 1 1 d . . . . .
C009 C 0.65439(19) 0.42870(14) 0.7982(3) 0.0177(5) Uani 1 1 d . . . . .
H00A H 0.6328 0.4175 0.9182 0.021 Uiso 1 1 calc R . . . .
H00B H 0.6256 0.4756 0.7657 0.021 Uiso 1 1 calc R . . . .
C00A C 0.9955(2) 0.37170(15) 0.6107(4) 0.0185(5) Uani 1 1 d . . . . .
C00B C 0.4994(2) 0.37375(14) 0.6556(4) 0.0175(5) Uani 1 1 d . . . . .
C00C C 0.4477(2) 0.38408(14) 0.5048(4) 0.0178(5) Uani 1 1 d . . . . .
C00D C 0.8012(2) 0.28499(14) 0.4188(4) 0.0203(6) Uani 1 1 d . . . . .
H00C H 0.7849 0.2861 0.2947 0.031 Uiso 1 1 calc GR . . . .
H00D H 0.7578 0.2499 0.4770 0.031 Uiso 1 1 calc GR . . . .
H00E H 0.8725 0.2717 0.4340 0.031 Uiso 1 1 calc GR . . . .
C00E C 0.7726(2) 0.43137(14) 0.7879(4) 0.0167(5) Uani 1 1 d . . . . .
H00F H 0.7936 0.4729 0.7146 0.020 Uiso 1 1 calc R . . . .
C00F C 0.8522(2) 0.41476(15) 0.4013(3) 0.0172(5) Uani 1 1 d . . . . .
H00G H 0.8394 0.4108 0.2750 0.021 Uiso 1 1 calc R . . . .
H00H H 0.8346 0.4638 0.4376 0.021 Uiso 1 1 calc R . . . .
C00G C 0.9259(2) 0.34937(15) 0.7318(4) 0.0183(5) Uani 1 1 d . . . . .
C00H C 0.9658(2) 0.40144(15) 0.4369(4) 0.0187(5) Uani 1 1 d . . . . .
C00I C 0.66585(19) 0.38453(14) 0.4884(3) 0.0157(5) Uani 1 1 d . . . . .
H00I H 0.6655 0.4373 0.4708 0.019 Uiso 1 1 calc R . . . .
C00J C 0.6511(2) 0.29723(15) 0.7464(4) 0.0212(6) Uani 1 1 d . . . . .
H00J H 0.6127 0.2863 0.8536 0.025 Uiso 1 1 calc R . . . .
H00K H 0.6377 0.2589 0.6611 0.025 Uiso 1 1 calc R . . . .
C00K C 0.6150(2) 0.37004(14) 0.6712(3) 0.0171(5) Uani 1 1 d . . . . .
C00L C 0.4251(2) 0.37054(16) 0.8093(4) 0.0203(5) Uani 1 1 d . . . . .
H00L H 0.4271 0.3234 0.8670 0.024 Uiso 1 1 calc R . . . .
H00M H 0.4400 0.4082 0.8957 0.024 Uiso 1 1 calc R . . . .
C00M C 0.81118(19) 0.35997(14) 0.7000(3) 0.0161(5) Uani 1 1 d . . . . .
C00N C 0.9619(2) 0.31426(16) 0.9015(4) 0.0226(6) Uani 1 1 d . . . . .
H00N H 0.9714 0.2631 0.8826 0.034 Uiso 1 1 calc GR . . . .
H00O H 0.9109 0.3217 0.9922 0.034 Uiso 1 1 calc GR . . . .
H00P H 1.0263 0.3357 0.9377 0.034 Uiso 1 1 calc GR . . . .
C00O C 0.4950(2) 0.38510(16) 0.3244(3) 0.0201(6) Uani 1 1 d . . . . .
H00Q H 0.4996 0.4347 0.2815 0.024 Uiso 1 1 calc R . . . .
H00R H 0.4523 0.3575 0.2427 0.024 Uiso 1 1 calc R . . . .
C00P C 0.78244(19) 0.36068(14) 0.4998(3) 0.0160(5) Uani 1 1 d . . . . .
C00Q C 0.6039(2) 0.35132(15) 0.3345(4) 0.0200(6) Uani 1 1 d . . . . .
H00S H 0.5981 0.2992 0.3514 0.024 Uiso 1 1 calc R . . . .
H00T H 0.6403 0.3598 0.2240 0.024 Uiso 1 1 calc R . . . .
O1 O 0.2472(3) 0.4143(2) 1.0675(4) 0.0555(10) Uani 0.796(5) 1 d . . . A 1
H1A H 0.2831 0.4503 1.1019 0.083 Uiso 0.796(5) 1 d G . . A 1
H1B H 0.2363 0.3859 1.1543 0.083 Uiso 0.796(5) 1 d G . . A 1
O1A O 0.2377(14) 0.3385(8) 1.0535(17) 0.0555(10) Uani 0.204(5) 1 d . . . A 2
H1AA H 0.1827 0.3462 0.9944 0.083 Uiso 0.204(5) 1 d G . . A 2
H1AB H 0.2893 0.3560 0.9982 0.083 Uiso 0.204(5) 1 d G . . A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O001 H001 0.8200 . ?
O001 C00E 1.421(3) . ?
O002 C00J 1.439(3) . ?
O002 C00M 1.440(3) . ?
O003 C008 1.249(3) . ?
O004 H00U 0.8500 . ?
O004 H00V 0.8501 . ?
O005 H005 0.8200 . ?
O005 C00A 1.358(3) . ?
O006 C00H 1.221(3) . ?
N007 H007 0.8600 . ?
N007 C008 1.345(4) . ?
N007 C00L 1.448(3) . ?
C008 C00C 1.483(3) . ?
C009 H00A 0.9700 . ?
C009 H00B 0.9700 . ?
C009 C00E 1.530(3) . ?
C009 C00K 1.530(4) . ?
C00A C00G 1.346(4) . ?
C00A C00H 1.472(4) . ?
C00B C00C 1.333(4) . ?
C00B C00K 1.499(4) . ?
C00B C00L 1.506(4) . ?
C00C C00O 1.493(4) . ?
C00D H00C 0.9600 . ?
C00D H00D 0.9600 . ?
C00D H00E 0.9600 . ?
C00D C00P 1.539(4) . ?
C00E H00F 0.9800 . ?
C00E C00M 1.552(4) . ?
C00F H00G 0.9700 . ?
C00F H00H 0.9700 . ?
C00F C00H 1.512(4) . ?
C00F C00P 1.534(3) . ?
C00G C00M 1.514(4) . ?
C00G C00N 1.507(4) . ?
C00I H00I 0.9800 . ?
C00I C00K 1.552(3) . ?
C00I C00P 1.571(4) . ?
C00I C00Q 1.537(4) . ?
C00J H00J 0.9700 . ?
C00J H00K 0.9700 . ?
C00J C00K 1.527(4) . ?
C00L H00L 0.9700 . ?
C00L H00M 0.9700 . ?
C00M C00P 1.556(3) . ?
C00N H00N 0.9600 . ?
C00N H00O 0.9600 . ?
C00N H00P 0.9600 . ?
C00O H00Q 0.9700 . ?
C00O H00R 0.9700 . ?
C00O C00Q 1.540(4) . ?
C00Q H00S 0.9700 . ?
C00Q H00T 0.9700 . ?
O1 H1A 0.8501 . ?
O1 H1B 0.8498 . ?
O1A H1AA 0.8497 . ?
O1A H1AB 0.8497 . ?

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
C00E O001 H001 109.5 . . ?
C00J O002 C00M 112.46(19) . . ?
H00U O004 H00V 109.5 . . ?
C00A O005 H005 109.5 . . ?
C008 N007 H007 123.8 . . ?
C008 N007 C00L 112.4(2) . . ?
C00L N007 H007 123.8 . . ?
O003 C008 N007 125.4(3) . . ?
O003 C008 C00C 127.6(3) . . ?
N007 C008 C00C 107.0(2) . . ?
H00A C009 H00B 108.3 . . ?
C00E C009 H00A 109.9 . . ?
C00E C009 H00B 109.9 . . ?
C00K C009 H00A 109.9 . . ?
C00K C009 H00B 109.9 . . ?
C00K C009 C00E 108.9(2) . . ?
O005 C00A C00H 115.9(2) . . ?
C00G C00A O005 120.9(2) . . ?
C00G C00A C00H 123.0(2) . . ?
C00C C00B C00K 124.9(2) . . ?
C00C C00B C00L 110.2(2) . . ?
C00K C00B C00L 124.9(2) . . ?
C008 C00C C00O 126.3(2) . . ?
C00B C00C C008 108.4(2) . . ?
C00B C00C C00O 125.2(2) . . ?
H00C C00D H00D 109.5 . . ?
H00C C00D H00E 109.5 . . ?
H00D C00D H00E 109.5 . . ?
C00P C00D H00C 109.5 . . ?
C00P C00D H00D 109.5 . . ?
C00P C00D H00E 109.5 . . ?
O001 C00E C009 107.6(2) . . ?
O001 C00E H00F 109.2 . . ?
O001 C00E C00M 113.2(2) . . ?
C009 C00E H00F 109.2 . . ?
C009 C00E C00M 108.3(2) . . ?
C00M C00E H00F 109.2 . . ?
H00G C00F H00H 107.9 . . ?
C00H C00F H00G 109.2 . . ?
C00H C00F H00H 109.2 . . ?
C00H C00F C00P 112.3(2) . . ?
C00P C00F H00G 109.2 . . ?
C00P C00F H00H 109.2 . . ?
C00A C00G C00M 120.4(2) . . ?
C00A C00G C00N 120.1(2) . . ?
C00N C00G C00M 119.4(2) . . ?
O006 C00H C00A 118.9(2) . . ?
O006 C00H C00F 122.9(2) . . ?
C00A C00H C00F 118.1(2) . . ?
C00K C00I H00I 106.8 . . ?
C00K C00I C00P 108.0(2) . . ?
C00P C00I H00I 106.8 . . ?
C00Q C00I H00I 106.8 . . ?
C00Q C00I C00K 112.6(2) . . ?
C00Q C00I C00P 115.4(2) . . ?
O002 C00J H00J 109.6 . . ?
O002 C00J H00K 109.6 . . ?
O002 C00J C00K 110.2(2) . . ?
H00J C00J H00K 108.1 . . ?
C00K C00J H00J 109.6 . . ?
C00K C00J H00K 109.6 . . ?
C009 C00K C00I 107.2(2) . . ?
C00B C00K C009 110.4(2) . . ?
C00B C00K C00I 110.1(2) . . ?
C00B C00K C00J 111.9(2) . . ?
C00J C00K C009 106.5(2) . . ?
C00J C00K C00I 110.6(2) . . ?
N007 C00L C00B 102.1(2) . . ?
N007 C00L H00L 111.4 . . ?
N007 C00L H00M 111.4 . . ?
C00B C00L H00L 111.4 . . ?
C00B C00L H00M 111.4 . . ?
H00L C00L H00M 109.2 . . ?
O002 C00M C00E 108.1(2) . . ?
O002 C00M C00G 106.2(2) . . ?
O002 C00M C00P 109.4(2) . . ?
C00E C00M C00P 109.3(2) . . ?
C00G C00M C00E 110.8(2) . . ?
C00G C00M C00P 112.9(2) . . ?
C00G C00N H00N 109.5 . . ?
C00G C00N H00O 109.5 . . ?
C00G C00N H00P 109.5 . . ?
H00N C00N H00O 109.5 . . ?
H00N C00N H00P 109.5 . . ?
H00O C00N H00P 109.5 . . ?
C00C C00O H00Q 109.9 . . ?
C00C C00O H00R 109.9 . . ?
C00C C00O C00Q 108.9(2) . . ?
H00Q C00O H00R 108.3 . . ?
C00Q C00O H00Q 109.9 . . ?
C00Q C00O H00R 109.9 . . ?
C00D C00P C00I 112.4(2) . . ?
C00D C00P C00M 109.9(2) . . ?
C00F C00P C00D 107.5(2) . . ?
C00F C00P C00I 110.8(2) . . ?
C00F C00P C00M 109.7(2) . . ?
C00M C00P C00I 106.52(19) . . ?
C00I C00Q C00O 110.7(2) . . ?
C00I C00Q H00S 109.5 . . ?
C00I C00Q H00T 109.5 . . ?
C00O C00Q H00S 109.5 . . ?
C00O C00Q H00T 109.5 . . ?
H00S C00Q H00T 108.1 . . ?
H1A O1 H1B 109.5 . . ?
H1AA O1A H1AB 109.5 . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.916
_oxdiff_exptl_absorpt_empirical_full_min 0.687
