 
data_20180124-7
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C28 H33 N O7' 
_chemical_formula_weight          495.55

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'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            154
_space_group_name_H-M_alt         'P 32 2 1'
_space_group_name_Hall            'P 32 2"'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z+2/3'
 '-x+y, -x, z+1/3'
 'y, x, -z'
 'x-y, -y, -z+1/3'
 '-x, -x+y, -z+2/3'
 
_cell_length_a                    20.0368(3)
_cell_length_b                    20.0368(3)
_cell_length_c                    12.7561(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      4435.09(14)
_cell_formula_units_Z             6
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     8648 
_cell_measurement_theta_min       0.812 
_cell_measurement_theta_max       0.976 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.113          
_exptl_crystal_F_000              1584
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.120
_exptl_crystal_size_mid           0.100
_exptl_crystal_size_min           0.100
_exptl_absorpt_coefficient_mu     0.655
_shelx_estimated_absorpt_T_min    0.926
_shelx_estimated_absorpt_T_max    0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min   0.914
_exptl_absorpt_correction_T_max   0.956
_exptl_absorpt_process_details   'SADABS, Sheldrick,2014'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Bruker APEX-II CCD' 
_diffrn_measurement_method        'φ and ω scans' 
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             17063
_diffrn_reflns_av_unetI/netI      0.0269
_diffrn_reflns_av_R_equivalents   0.0284
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -24
_diffrn_reflns_limit_k_max        23
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          2.546
_diffrn_reflns_theta_max          73.941
_diffrn_reflns_theta_full         67.679
_diffrn_measured_fraction_theta_max   0.985
_diffrn_measured_fraction_theta_full  0.997
_diffrn_reflns_Laue_measured_fraction_max    0.985
_diffrn_reflns_Laue_measured_fraction_full   0.997
_diffrn_reflns_point_group_measured_fraction_max   0.947
_diffrn_reflns_point_group_measured_fraction_full  0.974
_reflns_number_total              5687
_reflns_number_gt                 4968
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.768
_reflns_Friedel_fraction_max      0.902
_reflns_Friedel_fraction_full     0.947
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX2' 
_computing_cell_refinement        'Bruker SAINT' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'SHELXS-97 (Sheldrick 2008)' 
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1587P)²+0.5007P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.0035(6)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Flack x determined using 1925 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    -0.05(10)
_chemical_absolute_configuration   ad
_refine_ls_number_reflns          5687
_refine_ls_number_parameters      360
_refine_ls_number_restraints      30
_refine_ls_R_factor_all           0.0812
_refine_ls_R_factor_gt            0.0760
_refine_ls_wR_factor_ref          0.2023
_refine_ls_wR_factor_gt           0.1947
_refine_ls_goodness_of_fit_ref    0.976
_refine_ls_restrained_S_all       0.979
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C2 C 0.2528(2) 0.6771(2) 0.8090(3) 0.0515(7) Uani 1 1 d . . . . .
C3 C 0.2170(2) 0.7290(2) 0.8190(3) 0.0524(8) Uani 1 1 d . . . . .
C4 C 0.2057(2) 0.7427(2) 0.7061(3) 0.0537(8) Uani 1 1 d . . . . .
C5 C 0.1804(2) 0.7891(2) 0.6614(3) 0.0635(9) Uani 1 1 d . . . . .
H5 H 0.1650 0.8178 0.7042 0.076 Uiso 1 1 calc R U . . .
C6 C 0.1779(3) 0.7928(3) 0.5527(4) 0.0732(12) Uani 1 1 d . . . . .
H6 H 0.1604 0.8241 0.5206 0.088 Uiso 1 1 calc R U . . .
C7 C 0.2009(3) 0.7512(3) 0.4916(3) 0.0763(12) Uani 1 1 d . . . . .
H7 H 0.1983 0.7540 0.4175 0.092 Uiso 1 1 calc R U . . .
C8 C 0.2275(3) 0.7053(3) 0.5346(3) 0.0698(10) Uani 1 1 d . . . . .
H8 H 0.2435 0.6770 0.4919 0.084 Uiso 1 1 calc R U . . .
C9 C 0.2297(2) 0.7030(2) 0.6428(3) 0.0560(8) Uani 1 1 d . . . . .
C10 C 0.2788(2) 0.8017(2) 0.8764(3) 0.0557(8) Uani 1 1 d . . . . .
C11 C 0.2549(2) 0.8016(2) 0.9838(3) 0.0609(9) Uani 1 1 d . . . . .
C12 C 0.1808(3) 0.7458(2) 0.9929(3) 0.0630(9) Uani 1 1 d . . . . .
C13 C 0.1270(3) 0.7253(3) 1.0835(3) 0.0745(12) Uani 1 1 d . . . . .
H13A H 0.0867 0.7382 1.0658 0.089 Uiso 1 1 calc R U . . .
H13B H 0.1559 0.7570 1.1447 0.089 Uiso 1 1 calc R U . . .
C14 C 0.0879(2) 0.6395(3) 1.1143(3) 0.0667(10) Uani 1 1 d . . . . .
C15 C 0.1485(3) 0.6179(3) 1.1584(4) 0.0755(13) Uani 1 1 d . . . . .
H15 H 0.1888 0.6316 1.1033 0.091 Uiso 1 1 calc R U . . .
C16 C 0.1101(3) 0.5310(4) 1.1773(4) 0.0885(16) Uani 1 1 d . . . . .
H16A H 0.1487 0.5186 1.2054 0.106 Uiso 1 1 calc R U . . .
H16B H 0.0689 0.5154 1.2303 0.106 Uiso 1 1 calc R U . . .
C17 C 0.0766(2) 0.4864(3) 1.0793(4) 0.0757(12) Uani 1 1 d D . . . .
H17 H 0.1197 0.5047 1.0275 0.091 Uiso 1 1 calc R U . A 1
C18 C 0.0168(2) 0.5035(3) 1.0318(4) 0.0650(10) Uani 1 1 d . . . . .
H18 H -0.0009 0.4760 0.9631 0.078 Uiso 1 1 calc R U . . .
C19 C 0.0494(2) 0.5901(2) 1.0141(3) 0.0595(9) Uani 1 1 d . . . . .
C20 C 0.1046(2) 0.6136(2) 0.9197(3) 0.0553(8) Uani 1 1 d . . . . .
H20A H 0.1437 0.5984 0.9340 0.066 Uiso 1 1 calc R U . . .
H20B H 0.0748 0.5845 0.8573 0.066 Uiso 1 1 calc R U . . .
C21 C 0.1459(2) 0.6993(2) 0.8941(3) 0.0554(8) Uani 1 1 d . . . . .
C22 C 0.3075(3) 0.8576(3) 1.0636(3) 0.0727(11) Uani 1 1 d . . . . .
H22A H 0.2823 0.8445 1.1323 0.109 Uiso 1 1 calc R U . . .
H22B H 0.3198 0.9098 1.0440 0.109 Uiso 1 1 calc R U . . .
H22C H 0.3552 0.8552 1.0670 0.109 Uiso 1 1 calc R U . . .
C23 C 0.0303(3) 0.6292(4) 1.1998(4) 0.0837(14) Uani 1 1 d . . . . .
H23A H 0.0576 0.6635 1.2586 0.125 Uiso 1 1 calc R U . . .
H23B H 0.0037 0.5756 1.2240 0.125 Uiso 1 1 calc R U . . .
H23C H -0.0075 0.6419 1.1715 0.125 Uiso 1 1 calc R U . . .
C24 C 0.1888(3) 0.6608(5) 1.2564(4) 0.105(2) Uani 1 1 d . . . . .
H24A H 0.1518 0.6441 1.3143 0.157 Uiso 1 1 calc R U . . .
H24B H 0.2108 0.7162 1.2450 0.157 Uiso 1 1 calc R U . . .
H24C H 0.2301 0.6500 1.2737 0.157 Uiso 1 1 calc R U . . .
C1' C 0.0640(14) 0.3588(7) 1.0316(17) 0.073(3) Uani 0.502(7) 1 d D . P B 1
C2' C 0.0308(9) 0.2778(8) 1.0700(14) 0.092(4) Uani 0.502(7) 1 d D . P B 1
C5' C -0.0370(10) 0.2467(12) 1.135(2) 0.159(9) Uani 0.502(7) 1 d D U P B 1
H5'1 H -0.0850 0.2258 1.0975 0.239 Uiso 0.502(7) 1 d R U P B 1
H5'2 H -0.0309 0.2883 1.1786 0.239 Uiso 0.502(7) 1 d R U P B 1
H5'3 H -0.0368 0.2073 1.1770 0.239 Uiso 0.502(7) 1 d R U P B 1
C3' C 0.0574(11) 0.2305(8) 1.0352(14) 0.126(4) Uani 0.502(7) 1 d D . P B 1
H3' H 0.0229 0.1774 1.0479 0.152 Uiso 0.502(7) 1 calc R U P B 1
C4' C 0.1275(15) 0.2459(17) 0.983(2) 0.212(9) Uani 0.502(7) 1 d D . P B 1
H4'1 H 0.1232 0.2120 0.9270 0.317 Uiso 0.502(7) 1 d R U P B 1
H4'2 H 0.1606 0.2447 1.0367 0.317 Uiso 0.502(7) 1 d R U P B 1
H4'3 H 0.1489 0.2974 0.9568 0.317 Uiso 0.502(7) 1 d R U P B 1
O6 O 0.0454(11) 0.4028(5) 1.0922(17) 0.083(2) Uani 0.502(7) 1 d D . P B 1
O7 O 0.1217(6) 0.3885(7) 0.9743(8) 0.085(2) Uani 0.502(7) 1 d D . P B 1
C1" C 0.0505(16) 0.3631(7) 1.0576(14) 0.073(3) Uani 0.498(7) 1 d D . P B 2
C2" C 0.0052(9) 0.2807(8) 1.0925(12) 0.092(4) Uani 0.498(7) 1 d D . P B 2
C5" C -0.0129(6) 0.2675(7) 1.2021(11) 0.096(4) Uani 0.498(7) 1 d D U P B 2
H5"1 H -0.0375 0.2137 1.2193 0.144 Uiso 0.498(7) 1 d R U P B 2
H5"2 H -0.0466 0.2870 1.2196 0.144 Uiso 0.498(7) 1 d R U P B 2
H5"3 H 0.0341 0.2951 1.2412 0.144 Uiso 0.498(7) 1 d R U P B 2
C3" C -0.0146(12) 0.2214(7) 1.0234(13) 0.126(4) Uani 0.498(7) 1 d D . P B 2
H3" H -0.0436 0.1708 1.0514 0.152 Uiso 0.498(7) 1 calc R U P B 2
C4" C 0.004(2) 0.2265(16) 0.9124(18) 0.212(9) Uani 0.498(7) 1 d D . P B 2
H4"1 H 0.0069 0.2725 0.8840 0.317 Uiso 0.498(7) 1 d R U P B 2
H4"2 H -0.0322 0.1828 0.8717 0.317 Uiso 0.498(7) 1 d R U P B 2
H4"3 H 0.0534 0.2307 0.9102 0.317 Uiso 0.498(7) 1 d R U P B 2
O6' O 0.0329(11) 0.4068(6) 1.1172(17) 0.083(2) Uani 0.498(7) 1 d D . P B 2
O7' O 0.0851(6) 0.3821(7) 0.9743(8) 0.085(2) Uani 0.498(7) 1 d D . P B 2
N1 N 0.25649(18) 0.66302(18) 0.7054(2) 0.0544(7) Uani 1 1 d . . . . .
H1 H 0.2733 0.6331 0.6808 0.065 Uiso 1 1 calc R U . . .
O1 O 0.27692(16) 0.65496(17) 0.8813(2) 0.0588(6) Uani 1 1 d . . . . .
O2 O 0.33932(17) 0.84872(17) 0.8354(2) 0.0705(8) Uani 1 1 d . . . . .
O3 O -0.04769(16) 0.4797(2) 1.0982(3) 0.0749(9) Uani 1 1 d . . . . .
H3 H -0.0743 0.4313 1.0979 0.112 Uiso 1 1 calc R U . . .
O4 O -0.01476(16) 0.59893(18) 0.9822(2) 0.0659(7) Uani 1 1 d . . . . .
H4 H -0.0536 0.5699 1.0185 0.099 Uiso 1 1 calc R U . . .
O5 O 0.09345(16) 0.72191(17) 0.8551(2) 0.0634(7) Uani 1 1 d . . . . .
H5A H 0.0855 0.7111 0.7910 0.095 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
C2 O1 1.223(4) . ?
C2 N1 1.361(4) . ?
C2 C3 1.537(5) . ?
C3 C4 1.505(5) . ?
C3 C10 1.545(5) . ?
C3 C21 1.566(5) . ?
C4 C9 1.378(6) . ?
C4 C5 1.384(5) . ?
C5 C6 1.390(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.378(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.386(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(5) . ?
C8 H8 0.9500 . ?
C9 N1 1.414(5) . ?
C10 O2 1.220(5) . ?
C10 C11 1.451(5) . ?
C11 C12 1.346(6) . ?
C11 C22 1.492(5) . ?
C12 C13 1.491(6) . ?
C12 C21 1.514(5) . ?
C13 C14 1.542(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C23 1.525(6) . ?
C14 C19 1.563(6) . ?
C14 C15 1.583(7) . ?
C15 C24 1.502(7) . ?
C15 C16 1.532(9) . ?
C15 H15 1.0000 . ?
C16 C17 1.487(9) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 O6' 1.466(9) . ?
C17 O6 1.477(9) . ?
C17 C18 1.527(6) . ?
C17 H17 1.0000 . ?
C18 O3 1.413(5) . ?
C18 C19 1.535(6) . ?
C18 H18 1.0000 . ?
C19 O4 1.441(5) . ?
C19 C20 1.540(5) . ?
C20 C21 1.523(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 O5 1.425(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C1' O7 1.240(12) . ?
C1' O6 1.357(10) . ?
C1' C2' 1.496(14) . ?
C2' C3' 1.370(18) . ?
C2' C5' 1.437(15) . ?
C5' H5'1 0.9600 . ?
C5' H5'2 0.9600 . ?
C5' H5'3 0.9600 . ?
C3' C4' 1.442(17) . ?
C3' H3' 0.9500 . ?
C4' H4'1 0.9600 . ?
C4' H4'2 0.9600 . ?
C4' H4'3 0.9600 . ?
C1" O7' 1.221(11) . ?
C1" O6' 1.334(11) . ?
C1" C2" 1.498(14) . ?
C2" C3" 1.371(18) . ?
C2" C5" 1.436(16) . ?
C5" H5"1 0.9600 . ?
C5" H5"2 0.9600 . ?
C5" H5"3 0.9600 . ?
C3" C4" 1.452(16) . ?
C3" H3" 0.9500 . ?
C4" H4"1 0.9600 . ?
C4" H4"2 0.9600 . ?
C4" H4"3 0.9600 . ?
N1 H1 0.8800 . ?
O3 H3 0.8400 . ?
O4 H4 0.8400 . ?
O5 H5A 0.8400 . ?
 
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
O1 C2 N1 125.8(3) . . ?
O1 C2 C3 125.9(3) . . ?
N1 C2 C3 108.2(3) . . ?
C4 C3 C2 102.0(3) . . ?
C4 C3 C10 113.9(3) . . ?
C2 C3 C10 104.5(3) . . ?
C4 C3 C21 117.7(3) . . ?
C2 C3 C21 115.9(3) . . ?
C10 C3 C21 102.5(3) . . ?
C9 C4 C5 119.8(3) . . ?
C9 C4 C3 109.2(3) . . ?
C5 C4 C3 131.0(4) . . ?
C4 C5 C6 118.8(4) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C7 C6 C5 119.9(4) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 122.3(4) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C9 C8 C7 116.5(4) . . ?
C9 C8 H8 121.8 . . ?
C7 C8 H8 121.8 . . ?
C4 C9 C8 122.7(4) . . ?
C4 C9 N1 109.7(3) . . ?
C8 C9 N1 127.6(4) . . ?
O2 C10 C11 127.3(3) . . ?
O2 C10 C3 122.9(3) . . ?
C11 C10 C3 109.7(3) . . ?
C12 C11 C10 108.0(3) . . ?
C12 C11 C22 129.6(4) . . ?
C10 C11 C22 122.3(4) . . ?
C11 C12 C13 129.9(4) . . ?
C11 C12 C21 114.7(3) . . ?
C13 C12 C21 115.3(4) . . ?
C12 C13 C14 113.5(4) . . ?
C12 C13 H13A 108.9 . . ?
C14 C13 H13A 108.9 . . ?
C12 C13 H13B 108.9 . . ?
C14 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
C23 C14 C13 105.1(4) . . ?
C23 C14 C19 113.5(4) . . ?
C13 C14 C19 108.2(3) . . ?
C23 C14 C15 110.0(4) . . ?
C13 C14 C15 111.3(4) . . ?
C19 C14 C15 108.8(4) . . ?
C24 C15 C16 109.9(5) . . ?
C24 C15 C14 114.0(5) . . ?
C16 C15 C14 110.4(4) . . ?
C24 C15 H15 107.4 . . ?
C16 C15 H15 107.4 . . ?
C14 C15 H15 107.4 . . ?
C17 C16 C15 111.7(4) . . ?
C17 C16 H16A 109.3 . . ?
C15 C16 H16A 109.3 . . ?
C17 C16 H16B 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 107.9 . . ?
O6' C17 C16 102.7(10) . . ?
O6 C17 C16 113.3(10) . . ?
O6' C17 C18 105.4(10) . . ?
O6 C17 C18 111.3(10) . . ?
C16 C17 C18 111.7(5) . . ?
O6 C17 H17 106.7 . . ?
C16 C17 H17 106.7 . . ?
C18 C17 H17 106.7 . . ?
O3 C18 C17 112.0(3) . . ?
O3 C18 C19 105.7(4) . . ?
C17 C18 C19 111.9(3) . . ?
O3 C18 H18 109.1 . . ?
C17 C18 H18 109.1 . . ?
C19 C18 H18 109.1 . . ?
O4 C19 C18 106.2(3) . . ?
O4 C19 C20 106.8(3) . . ?
C18 C19 C20 107.2(3) . . ?
O4 C19 C14 109.9(3) . . ?
C18 C19 C14 113.0(3) . . ?
C20 C19 C14 113.2(3) . . ?
C21 C20 C19 114.5(3) . . ?
C21 C20 H20A 108.6 . . ?
C19 C20 H20A 108.6 . . ?
C21 C20 H20B 108.6 . . ?
C19 C20 H20B 108.6 . . ?
H20A C20 H20B 107.6 . . ?
O5 C21 C12 106.4(3) . . ?
O5 C21 C20 111.2(3) . . ?
C12 C21 C20 109.8(3) . . ?
O5 C21 C3 109.9(3) . . ?
C12 C21 C3 102.9(3) . . ?
C20 C21 C3 116.0(3) . . ?
C11 C22 H22A 109.5 . . ?
C11 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C11 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C14 C23 H23A 109.5 . . ?
C14 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C14 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C15 C24 H24A 109.5 . . ?
C15 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C15 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O7 C1' O6 121.1(11) . . ?
O7 C1' C2' 121.0(12) . . ?
O6 C1' C2' 113.7(10) . . ?
C3' C2' C5' 119.7(12) . . ?
C3' C2' C1' 121.9(11) . . ?
C5' C2' C1' 117.9(11) . . ?
C2' C5' H5'1 115.5 . . ?
C2' C5' H5'2 106.1 . . ?
H5'1 C5' H5'2 109.5 . . ?
C2' C5' H5'3 106.7 . . ?
H5'1 C5' H5'3 109.5 . . ?
H5'2 C5' H5'3 109.5 . . ?
C2' C3' C4' 132.5(16) . . ?
C2' C3' H3' 113.7 . . ?
C4' C3' H3' 113.7 . . ?
C3' C4' H4'1 117.4 . . ?
C3' C4' H4'2 106.1 . . ?
H4'1 C4' H4'2 109.5 . . ?
C3' C4' H4'3 104.6 . . ?
H4'1 C4' H4'3 109.5 . . ?
H4'2 C4' H4'3 109.5 . . ?
C1' O6 C17 125.2(8) . . ?
O7' C1" O6' 125.8(11) . . ?
O7' C1" C2" 122.6(11) . . ?
O6' C1" C2" 109.9(11) . . ?
C3" C2" C5" 122.0(11) . . ?
C3" C2" C1" 121.2(12) . . ?
C5" C2" C1" 116.8(11) . . ?
C2" C5" H5"1 111.7 . . ?
C2" C5" H5"2 108.4 . . ?
H5"1 C5" H5"2 109.5 . . ?
C2" C5" H5"3 108.3 . . ?
H5"1 C5" H5"3 109.5 . . ?
H5"2 C5" H5"3 109.5 . . ?
C2" C3" C4" 127.8(15) . . ?
C2" C3" H3" 116.1 . . ?
C4" C3" H3" 116.1 . . ?
C3" C4" C4" 164(4) . 6_556 ?
C3" C4" H4"1 109.3 . . ?
C4" C4" H4"1 68.1 6_556 . ?
C3" C4" H4"2 114.7 . . ?
C4" C4" H4"2 54.6 6_556 . ?
H4"1 C4" H4"2 109.5 . . ?
C3" C4" H4"3 104.3 . . ?
C4" C4" H4"3 91.5 6_556 . ?
H4"1 C4" H4"3 109.5 . . ?
H4"2 C4" H4"3 109.5 . . ?
C1" O6' C17 108.5(8) . . ?
C2 N1 C9 110.8(3) . . ?
C2 N1 H1 124.6 . . ?
C9 N1 H1 124.6 . . ?
C18 O3 H3 109.5 . . ?
C19 O4 H4 109.5 . . ?
C21 O5 H5A 109.5 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
O1 C2 C3 C4 174.7(3) . . . . ?
N1 C2 C3 C4 -2.3(4) . . . . ?
O1 C2 C3 C10 55.9(4) . . . . ?
N1 C2 C3 C10 -121.1(3) . . . . ?
O1 C2 C3 C21 -56.2(5) . . . . ?
N1 C2 C3 C21 126.8(3) . . . . ?
C2 C3 C4 C9 1.3(4) . . . . ?
C10 C3 C4 C9 113.3(3) . . . . ?
C21 C3 C4 C9 -126.7(3) . . . . ?
C2 C3 C4 C5 -175.2(4) . . . . ?
C10 C3 C4 C5 -63.2(5) . . . . ?
C21 C3 C4 C5 56.8(5) . . . . ?
C9 C4 C5 C6 1.6(6) . . . . ?
C3 C4 C5 C6 177.8(4) . . . . ?
C4 C5 C6 C7 -0.4(7) . . . . ?
C5 C6 C7 C8 -0.6(8) . . . . ?
C6 C7 C8 C9 0.3(7) . . . . ?
C5 C4 C9 C8 -2.0(6) . . . . ?
C3 C4 C9 C8 -178.9(4) . . . . ?
C5 C4 C9 N1 177.0(3) . . . . ?
C3 C4 C9 N1 0.1(4) . . . . ?
C7 C8 C9 C4 1.0(6) . . . . ?
C7 C8 C9 N1 -177.8(4) . . . . ?
C4 C3 C10 O2 -39.8(5) . . . . ?
C2 C3 C10 O2 70.7(5) . . . . ?
C21 C3 C10 O2 -168.0(4) . . . . ?
C4 C3 C10 C11 143.1(3) . . . . ?
C2 C3 C10 C11 -106.5(3) . . . . ?
C21 C3 C10 C11 14.9(4) . . . . ?
O2 C10 C11 C12 172.0(4) . . . . ?
C3 C10 C11 C12 -11.0(5) . . . . ?
O2 C10 C11 C22 -6.6(7) . . . . ?
C3 C10 C11 C22 170.4(4) . . . . ?
C10 C11 C12 C13 -174.8(5) . . . . ?
C22 C11 C12 C13 3.7(8) . . . . ?
C10 C11 C12 C21 2.0(5) . . . . ?
C22 C11 C12 C21 -179.5(4) . . . . ?
C11 C12 C13 C14 -127.4(5) . . . . ?
C21 C12 C13 C14 55.8(5) . . . . ?
C12 C13 C14 C23 -174.6(4) . . . . ?
C12 C13 C14 C19 -53.0(5) . . . . ?
C12 C13 C14 C15 66.4(5) . . . . ?
C23 C14 C15 C24 -54.2(6) . . . . ?
C13 C14 C15 C24 61.9(5) . . . . ?
C19 C14 C15 C24 -179.0(4) . . . . ?
C23 C14 C15 C16 70.1(5) . . . . ?
C13 C14 C15 C16 -173.9(4) . . . . ?
C19 C14 C15 C16 -54.8(5) . . . . ?
C24 C15 C16 C17 -174.0(4) . . . . ?
C14 C15 C16 C17 59.4(5) . . . . ?
C15 C16 C17 O6' -171.2(8) . . . . ?
C15 C16 C17 O6 174.7(7) . . . . ?
C15 C16 C17 C18 -58.7(5) . . . . ?
O6' C17 C18 O3 46.8(9) . . . . ?
O6 C17 C18 O3 63.7(8) . . . . ?
C16 C17 C18 O3 -64.1(5) . . . . ?
O6' C17 C18 C19 165.3(7) . . . . ?
O6 C17 C18 C19 -177.8(7) . . . . ?
C16 C17 C18 C19 54.4(5) . . . . ?
O3 C18 C19 O4 -50.7(4) . . . . ?
C17 C18 C19 O4 -172.8(4) . . . . ?
O3 C18 C19 C20 -164.6(3) . . . . ?
C17 C18 C19 C20 73.2(5) . . . . ?
O3 C18 C19 C14 69.9(4) . . . . ?
C17 C18 C19 C14 -52.2(5) . . . . ?
C23 C14 C19 O4 47.8(5) . . . . ?
C13 C14 C19 O4 -68.4(4) . . . . ?
C15 C14 C19 O4 170.5(3) . . . . ?
C23 C14 C19 C18 -70.7(5) . . . . ?
C13 C14 C19 C18 173.1(3) . . . . ?
C15 C14 C19 C18 52.1(4) . . . . ?
C23 C14 C19 C20 167.2(4) . . . . ?
C13 C14 C19 C20 50.9(5) . . . . ?
C15 C14 C19 C20 -70.1(4) . . . . ?
O4 C19 C20 C21 69.6(4) . . . . ?
C18 C19 C20 C21 -176.9(3) . . . . ?
C14 C19 C20 C21 -51.6(5) . . . . ?
C11 C12 C21 O5 -108.1(4) . . . . ?
C13 C12 C21 O5 69.2(5) . . . . ?
C11 C12 C21 C20 131.5(4) . . . . ?
C13 C12 C21 C20 -51.3(5) . . . . ?
C11 C12 C21 C3 7.4(5) . . . . ?
C13 C12 C21 C3 -175.3(4) . . . . ?
C19 C20 C21 O5 -68.6(4) . . . . ?
C19 C20 C21 C12 48.9(4) . . . . ?
C19 C20 C21 C3 164.9(3) . . . . ?
C4 C3 C21 O5 -25.5(4) . . . . ?
C2 C3 C21 O5 -146.5(3) . . . . ?
C10 C3 C21 O5 100.3(3) . . . . ?
C4 C3 C21 C12 -138.5(3) . . . . ?
C2 C3 C21 C12 100.5(3) . . . . ?
C10 C3 C21 C12 -12.7(4) . . . . ?
C4 C3 C21 C20 101.7(4) . . . . ?
C2 C3 C21 C20 -19.4(5) . . . . ?
C10 C3 C21 C20 -132.6(3) . . . . ?
O7 C1' C2' C3' -7(4) . . . . ?
O6 C1' C2' C3' -164(2) . . . . ?
O7 C1' C2' C5' -179(2) . . . . ?
O6 C1' C2' C5' 24(4) . . . . ?
C5' C2' C3' C4' -170(3) . . . . ?
C1' C2' C3' C4' 18(4) . . . . ?
O7 C1' O6 C17 16(5) . . . . ?
C2' C1' O6 C17 173.3(19) . . . . ?
C16 C17 O6 C1' -127(3) . . . . ?
C18 C17 O6 C1' 106(3) . . . . ?
O7' C1" C2" C3" -15(4) . . . . ?
O6' C1" C2" C3" 151(2) . . . . ?
O7' C1" C2" C5" 162(2) . . . . ?
O6' C1" C2" C5" -32(3) . . . . ?
C5" C2" C3" C4" -176(2) . . . . ?
C1" C2" C3" C4" 0(4) . . . . ?
C2" C3" C4" C4" -108(5) . . . 6_556 ?
O7' C1" O6' C17 -13(4) . . . . ?
C2" C1" O6' C17 -178.5(17) . . . . ?
C16 C17 O6' C1" -132(2) . . . . ?
C18 C17 O6' C1" 111(2) . . . . ?
O1 C2 N1 C9 -174.5(3) . . . . ?
C3 C2 N1 C9 2.5(4) . . . . ?
C4 C9 N1 C2 -1.6(4) . . . . ?
C8 C9 N1 C2 177.3(4) . . . . ?
 
loop_
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
O4 H4 O3  0.84 2.13 2.600(4) 115.2 .
O3 H3 O2  0.84 1.91 2.664(4) 148.3 4_457
N1 H1 O1  0.88 2.30 3.053(4) 143.1 2_664
C20 H20A O1  0.99 2.42 3.161(5) 131.6 .
 
_refine_diff_density_max    0.678
_refine_diff_density_min   -0.335
_refine_diff_density_rms    0.129

_vrf_PLAT602_20180124-7
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: Due to the serious disorder of the solvent molecules, these 
solvent molecules have been squeezed in the final refinement by using
PLATON/SQUEEZE program. This alert can be omitted.
;




