 
data_A20002_014
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C15 H18 Cl3 N O5' 
_chemical_formula_weight          398.65

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    12.9773(19)
_cell_length_b                    14.749(2)
_cell_length_c                    11.1908(17)
_cell_angle_alpha                 90
_cell_angle_beta                  115.237(4)
_cell_angle_gamma                 90
_cell_volume                      1937.5(5)
_cell_formula_units_Z             4
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used      9767
_cell_measurement_theta_min        3.17
_cell_measurement_theta_max       26.14
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'colourless'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.367          
_exptl_crystal_F_000              824
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.344
_exptl_crystal_size_mid           0.221
_exptl_crystal_size_min           0.078
_exptl_absorpt_coefficient_mu     0.495
_shelx_estimated_absorpt_T_min    0.848
_shelx_estimated_absorpt_T_max    0.962
_exptl_absorpt_correction_type    MULTI-SCAN
_exptl_absorpt_correction_T_min   0.6551
_exptl_absorpt_correction_T_max   0.7454
_exptl_absorpt_process_details    SADABS 
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'
_diffrn_measurement_device_type   'Bruker PHOTON II'  
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             83371
_diffrn_reflns_av_unetI/netI      0.0239
_diffrn_reflns_av_R_equivalents   0.0821
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          2.440
_diffrn_reflns_theta_max          24.990
_diffrn_reflns_theta_full         24.990
_diffrn_measured_fraction_theta_max   0.986
_diffrn_measured_fraction_theta_full  0.986
_diffrn_reflns_Laue_measured_fraction_max    0.986
_diffrn_reflns_Laue_measured_fraction_full   0.986
_diffrn_reflns_point_group_measured_fraction_max   0.986
_diffrn_reflns_point_group_measured_fraction_full  0.986
_reflns_number_total              3362
_reflns_number_gt                 2544
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEXIII' 
_computing_cell_refinement        'Bruker APEXIII' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     SHELXS
_computing_structure_refinement   SHELXL
_computing_molecular_graphics     ORTEP
_computing_publication_material   CIFTAB
_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)+(0.0594P)²+3.2328P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          3362
_refine_ls_number_parameters      279
_refine_ls_number_restraints      365
_refine_ls_R_factor_all           0.1151
_refine_ls_R_factor_gt            0.0874
_refine_ls_wR_factor_ref          0.2194
_refine_ls_wR_factor_gt           0.1901
_refine_ls_goodness_of_fit_ref    1.138
_refine_ls_restrained_S_all       1.141
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.6743(7) 0.5446(6) 0.1643(9) 0.061(2) Uani 0.728(7) 1 d D U P A 1
H1A H 0.672429 0.610225 0.157997 0.074 Uiso 0.728(7) 1 calc R U P A 1
H1AB H 0.624483 0.520776 0.078058 0.074 Uiso 0.728(7) 1 calc R U P A 1
C2 C 0.7926(7) 0.5131(5) 0.1990(8) 0.075(2) Uani 0.728(7) 1 d D U P A 1
Cl3 Cl 0.8252(5) 0.5487(4) 0.0676(5) 0.1148(16) Uani 0.728(7) 1 d D U P A 1
Cl4 Cl 0.8017(3) 0.39402(16) 0.2122(4) 0.1060(12) Uani 0.728(7) 1 d D U P A 1
Cl5 Cl 0.8891(3) 0.5594(4) 0.3485(3) 0.1446(16) Uani 0.728(7) 1 d D U P A 1
C1B C 0.6668(16) 0.519(2) 0.145(3) 0.077(5) Uani 0.272(7) 1 d D U P A 2
H1BA H 0.648193 0.463102 0.095390 0.092 Uiso 0.272(7) 1 calc R U P A 2
H1BB H 0.634794 0.570263 0.086384 0.092 Uiso 0.272(7) 1 calc R U P A 2
C2B C 0.7902(17) 0.5293(12) 0.2270(18) 0.088(5) Uani 0.272(7) 1 d D U P A 2
Cl3B Cl 0.8630(13) 0.5451(13) 0.1274(15) 0.131(4) Uani 0.272(7) 1 d D U P A 2
Cl4B Cl 0.8477(10) 0.4316(11) 0.3180(17) 0.191(6) Uani 0.272(7) 1 d D U P A 2
Cl5B Cl 0.8245(14) 0.6247(10) 0.3262(14) 0.195(6) Uani 0.272(7) 1 d D U P A 2
O6 O 0.6317(3) 0.5181(2) 0.2565(3) 0.0648(8) Uani 1 1 d . U . . .
C7 C 0.5556(3) 0.4493(3) 0.2292(4) 0.0519(9) Uani 1 1 d . U . . .
O8 O 0.5227(3) 0.4044(2) 0.1307(3) 0.0743(9) Uani 1 1 d . U . . .
N9 N 0.5210(3) 0.4419(2) 0.3248(3) 0.0515(8) Uani 1 1 d . U . . .
H9 H 0.547(4) 0.477(3) 0.389(4) 0.062 Uiso 1 1 d . U . . .
C10 C 0.4516(3) 0.3676(2) 0.3325(4) 0.0488(9) Uani 1 1 d . U . . .
H10 H 0.425673 0.331676 0.251245 0.059 Uiso 1 1 calc R U . . .
C11 C 0.3486(4) 0.4051(3) 0.3480(4) 0.0545(10) Uani 1 1 d . U . . .
O12 O 0.3530(3) 0.4649(2) 0.4209(3) 0.0781(10) Uani 1 1 d . U . . .
O13 O 0.2545(3) 0.3636(3) 0.2714(4) 0.0871(11) Uani 1 1 d D U . . .
C14 C 0.1451(11) 0.3831(13) 0.2775(16) 0.104(4) Uani 0.66(3) 1 d D U P B 1
H14A H 0.081647 0.370191 0.193274 0.125 Uiso 0.66(3) 1 calc R U P B 1
H14B H 0.141341 0.446315 0.299314 0.125 Uiso 0.66(3) 1 calc R U P B 1
C15 C 0.1413(18) 0.3229(12) 0.383(2) 0.141(6) Uani 0.66(3) 1 d D U P B 1
H15A H 0.073893 0.335786 0.395022 0.211 Uiso 0.66(3) 1 calc R U P B 1
H15B H 0.207382 0.333628 0.464079 0.211 Uiso 0.66(3) 1 calc R U P B 1
H15C H 0.140250 0.260709 0.357199 0.211 Uiso 0.66(3) 1 calc R U P B 1
C14B C 0.165(2) 0.394(2) 0.313(4) 0.103(6) Uani 0.34(3) 1 d D U P B 2
H14C H 0.119658 0.443543 0.257789 0.124 Uiso 0.34(3) 1 calc R U P B 2
H14D H 0.197292 0.412976 0.404628 0.124 Uiso 0.34(3) 1 calc R U P B 2
C15B C 0.095(2) 0.3088(18) 0.291(5) 0.128(8) Uani 0.34(3) 1 d D U P B 2
H15D H 0.023263 0.322986 0.291519 0.192 Uiso 0.34(3) 1 calc R U P B 2
H15E H 0.135607 0.266461 0.360748 0.192 Uiso 0.34(3) 1 calc R U P B 2
H15F H 0.083067 0.282546 0.207737 0.192 Uiso 0.34(3) 1 calc R U P B 2
C16 C 0.5203(4) 0.3066(3) 0.4517(4) 0.0557(10) Uani 1 1 d . U . . .
H16 H 0.550337 0.344253 0.531428 0.067 Uiso 1 1 calc R U . . .
O17 O 0.4425(3) 0.2451(2) 0.4615(3) 0.0777(10) Uani 1 1 d D U . . .
H17 H 0.478(5) 0.205(3) 0.528(4) 0.117 Uiso 1 1 d D U . . .
C18 C 0.6197(2) 0.26329(17) 0.4362(3) 0.0536(10) Uani 1 1 d G U . . .
C19 C 0.7282(2) 0.29992(17) 0.5021(3) 0.0703(12) Uani 1 1 d G U . . .
H19 H 0.739724 0.349871 0.557068 0.084 Uiso 1 1 calc R U . . .
C20 C 0.81941(19) 0.2619(2) 0.4859(3) 0.0820(14) Uani 1 1 d G U . . .
H20 H 0.891984 0.286385 0.530032 0.098 Uiso 1 1 calc R U . . .
C21 C 0.8022(2) 0.1872(2) 0.4038(3) 0.0788(14) Uani 1 1 d G U . . .
C22 C 0.6937(3) 0.15059(18) 0.3378(3) 0.0765(13) Uani 1 1 d G U . . .
H22 H 0.682151 0.100638 0.282891 0.092 Uiso 1 1 calc R U . . .
C23 C 0.6025(2) 0.18863(18) 0.3540(3) 0.0659(11) Uani 1 1 d G U . . .
H23 H 0.529889 0.164122 0.309926 0.079 Uiso 1 1 calc R U . . .
C24 C 0.9016(5) 0.1448(5) 0.3874(7) 0.114(2) Uani 1 1 d . U . . .
H24A H 0.900976 0.080412 0.399289 0.171 Uiso 1 1 calc R U . . .
H24B H 0.971644 0.169577 0.452108 0.171 Uiso 1 1 calc R U . . .
H24C H 0.895397 0.157655 0.300477 0.171 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
C1 O6 1.418(11) . ?
C1 C2 1.488(10) . ?
C1 H1A 0.9700 . ?
C1 H1AB 0.9700 . ?
C2 Cl5 1.746(8) . ?
C2 Cl4 1.762(8) . ?
C2 Cl3 1.774(8) . ?
C1B C2B 1.474(17) . ?
C1B O6 1.50(3) . ?
C1B H1BA 0.9700 . ?
C1B H1BB 0.9700 . ?
C2B Cl5B 1.730(17) . ?
C2B Cl4B 1.737(17) . ?
C2B Cl3B 1.757(16) . ?
O6 C7 1.357(5) . ?
C7 O8 1.198(5) . ?
C7 N9 1.329(5) . ?
N9 C10 1.443(5) . ?
N9 H9 0.83(4) . ?
C10 C11 1.523(6) . ?
C10 C16 1.539(5) . ?
C10 H10 0.9800 . ?
C11 O12 1.186(5) . ?
C11 O13 1.307(5) . ?
O13 C14 1.478(12) . ?
O13 C14B 1.496(18) . ?
C14 C15 1.493(15) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C14B C15B 1.507(19) . ?
C14B H14C 0.9700 . ?
C14B H14D 0.9700 . ?
C15B H15D 0.9600 . ?
C15B H15E 0.9600 . ?
C15B H15F 0.9600 . ?
C16 O17 1.397(5) . ?
C16 C18 1.514(5) . ?
C16 H16 0.9800 . ?
O17 H17 0.91(2) . ?
C18 C19 1.3900 . ?
C18 C23 1.3900 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 H20 0.9300 . ?
C21 C22 1.3900 . ?
C21 C24 1.514(6) . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 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
O6 C1 C2 113.8(7) . . ?
O6 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
O6 C1 H1AB 108.8 . . ?
C2 C1 H1AB 108.8 . . ?
H1A C1 H1AB 107.7 . . ?
C1 C2 Cl5 111.4(6) . . ?
C1 C2 Cl4 111.0(6) . . ?
Cl5 C2 Cl4 108.3(5) . . ?
C1 C2 Cl3 106.0(6) . . ?
Cl5 C2 Cl3 110.6(4) . . ?
Cl4 C2 Cl3 109.5(5) . . ?
C2B C1B O6 96.9(18) . . ?
C2B C1B H1BA 112.4 . . ?
O6 C1B H1BA 112.4 . . ?
C2B C1B H1BB 112.4 . . ?
O6 C1B H1BB 112.4 . . ?
H1BA C1B H1BB 109.9 . . ?
C1B C2B Cl5B 113.2(17) . . ?
C1B C2B Cl4B 111.2(16) . . ?
Cl5B C2B Cl4B 111.7(12) . . ?
C1B C2B Cl3B 110.8(17) . . ?
Cl5B C2B Cl3B 103.8(11) . . ?
Cl4B C2B Cl3B 105.6(12) . . ?
C7 O6 C1 121.0(4) . . ?
C7 O6 C1B 105.8(10) . . ?
O8 C7 N9 125.8(4) . . ?
O8 C7 O6 124.0(4) . . ?
N9 C7 O6 110.2(3) . . ?
C7 N9 C10 123.0(3) . . ?
C7 N9 H9 119(3) . . ?
C10 N9 H9 117(3) . . ?
N9 C10 C11 109.3(3) . . ?
N9 C10 C16 110.5(3) . . ?
C11 C10 C16 109.0(3) . . ?
N9 C10 H10 109.3 . . ?
C11 C10 H10 109.3 . . ?
C16 C10 H10 109.3 . . ?
O12 C11 O13 123.8(4) . . ?
O12 C11 C10 124.1(4) . . ?
O13 C11 C10 112.1(4) . . ?
C11 O13 C14 121.8(8) . . ?
C11 O13 C14B 106.8(12) . . ?
O13 C14 C15 106.0(12) . . ?
O13 C14 H14A 110.5 . . ?
C15 C14 H14A 110.5 . . ?
O13 C14 H14B 110.5 . . ?
C15 C14 H14B 110.5 . . ?
H14A C14 H14B 108.7 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O13 C14B C15B 100.8(19) . . ?
O13 C14B H14C 111.6 . . ?
C15B C14B H14C 111.6 . . ?
O13 C14B H14D 111.6 . . ?
C15B C14B H14D 111.6 . . ?
H14C C14B H14D 109.4 . . ?
C14B C15B H15D 109.5 . . ?
C14B C15B H15E 109.5 . . ?
H15D C15B H15E 109.5 . . ?
C14B C15B H15F 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
O17 C16 C18 114.5(3) . . ?
O17 C16 C10 106.1(3) . . ?
C18 C16 C10 110.8(3) . . ?
O17 C16 H16 108.4 . . ?
C18 C16 H16 108.4 . . ?
C10 C16 H16 108.4 . . ?
C16 O17 H17 111(4) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C16 119.6(2) . . ?
C23 C18 C16 120.3(2) . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 120.0 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 120.0 . . ?
C22 C21 C24 119.9(4) . . ?
C20 C21 C24 120.1(4) . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C18 120.0 . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 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
O6 C1 C2 Cl5 -62.4(8) . . . . ?
O6 C1 C2 Cl4 58.4(8) . . . . ?
O6 C1 C2 Cl3 177.2(5) . . . . ?
O6 C1B C2B Cl5B -57.8(19) . . . . ?
O6 C1B C2B Cl4B 68.9(19) . . . . ?
O6 C1B C2B Cl3B -174.0(13) . . . . ?
C2 C1 O6 C7 -103.9(7) . . . . ?
C2B C1B O6 C7 -135.0(13) . . . . ?
C1 O6 C7 O8 3.1(7) . . . . ?
C1B O6 C7 O8 -3.3(11) . . . . ?
C1 O6 C7 N9 -174.8(5) . . . . ?
C1B O6 C7 N9 178.8(10) . . . . ?
O8 C7 N9 C10 10.5(6) . . . . ?
O6 C7 N9 C10 -171.6(3) . . . . ?
C7 N9 C10 C11 -128.7(4) . . . . ?
C7 N9 C10 C16 111.3(4) . . . . ?
N9 C10 C11 O12 -44.5(5) . . . . ?
C16 C10 C11 O12 76.4(5) . . . . ?
N9 C10 C11 O13 135.5(4) . . . . ?
C16 C10 C11 O13 -103.6(4) . . . . ?
O12 C11 O13 C14 -5.2(10) . . . . ?
C10 C11 O13 C14 174.8(9) . . . . ?
O12 C11 O13 C14B -10.0(18) . . . . ?
C10 C11 O13 C14B 170.0(17) . . . . ?
C11 O13 C14 C15 -86.6(19) . . . . ?
C11 O13 C14B C15B -145(3) . . . . ?
N9 C10 C16 O17 171.9(3) . . . . ?
C11 C10 C16 O17 51.8(4) . . . . ?
N9 C10 C16 C18 -63.3(4) . . . . ?
C11 C10 C16 C18 176.6(3) . . . . ?
O17 C16 C18 C19 -140.3(3) . . . . ?
C10 C16 C18 C19 99.8(3) . . . . ?
O17 C16 C18 C23 41.3(4) . . . . ?
C10 C16 C18 C23 -78.6(3) . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
C16 C18 C19 C20 -178.4(3) . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C19 C20 C21 C24 -179.2(4) . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C24 C21 C22 C23 179.2(4) . . . . ?
C21 C22 C23 C18 0.0 . . . . ?
C19 C18 C23 C22 0.0 . . . . ?
C16 C18 C23 C22 178.4(3) . . . . ?
 
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 
 _geom_hbond_publ_flag
N9 H9 O12  0.83(4) 2.14(5) 2.949(5) 164(4) 3_666 yes
O17 H17 O8  0.91(2) 1.92(3) 2.801(4) 163(6) 4_566 yes
 
_refine_diff_density_max    0.477
_refine_diff_density_min   -0.397
_refine_diff_density_rms    0.049


