 
data_compound1.cif 
 
_publ_contact_author
;
Packianathan Thomas Muthiah
Department of Chemistry,
Bharathidasan University,
Tiruchirappalli-640 024
India.
;
_publ_contact_author_phone        '91-431-2407053'
_publ_contact_author_fax         
_publ_contact_author_email        'tommtrichy@yahoo.co.in'

loop_
 _publ_author_name
 _publ_author_address
 'Savarimuthu Francis'
;
Department of Chemistry,
Bharathidasan University,
Tiruchirappalli-620 024
India
;

 'Packianathan Thomas Muthiah'
;
Department of Chemistry,
Bharathidasan University,
Tiruchirappalli-620 024
India
;
 'Rychlewska, Urszula'
;
Department of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Poznań
Poland
;
 'Warżajtis, Beata'
;
Department of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Poznań
Poland
;
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             'Trimethoprim hydrogen Phthalate' 
_chemical_melting_point           ? 
_chemical_formula_moiety          '(C14 H19 N4 O3), (C8 H5 O4)'
_chemical_formula_sum 
 'C22 H24 N4 O7' 
_chemical_formula_weight          456.45 
 
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' 
 
_symmetry_cell_setting            triclinic 
_symmetry_space_group_name_H-M    'P -1' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    4.6510(10) 
_cell_length_b                    11.700(2) 
_cell_length_c                    20.362(4) 
_cell_angle_alpha                 76.21(3) 
_cell_angle_beta                  86.23(3) 
_cell_angle_gamma                 84.03(3) 
_cell_volume                      1069.3(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     61
_cell_measurement_theta_min       5.20 
_cell_measurement_theta_max       27.81 
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.30 
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.418 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              480 
_exptl_absorpt_coefficient_mu     0.900 
_exptl_absorpt_correction_type    'PSI SCAN' 
_exptl_absorpt_correction_T_min   0.474 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'KM-4 four circle diffractometer'
_diffrn_measurement_method        'Θ--2Θ'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          2 
_diffrn_standards_interval_count  100 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0.8
_diffrn_reflns_number             4420 
_diffrn_reflns_av_R_equivalents   0.0278 
_diffrn_reflns_av_sigmaI/netI     0.0193 
_diffrn_reflns_limit_h_min        -5 
_diffrn_reflns_limit_h_max        5 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          2.24 
_diffrn_reflns_theta_max          67.10 
_reflns_number_total              3802 
_reflns_number_gt                 3138 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Kuma KM-4 software (Kuma Diffraction, 1991)'
_computing_cell_refinement        'Kuma KM-4 software (Kuma Diffraction, 1991)'
_computing_data_reduction         'Kuma KM-4 software (Kuma Diffraction, 1991)'
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0825P)²+0.1217P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0196(14)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          3802
_refine_ls_number_parameters      395
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0533
_refine_ls_R_factor_gt            0.0421
_refine_ls_wR_factor_ref          0.1245
_refine_ls_wR_factor_gt           0.1182
_refine_ls_goodness_of_fit_ref    1.070
_refine_ls_restrained_S_all       1.070
_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_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
N2 N 0.6328(3) 0.28523(13) 0.46335(8) 0.0549(4) Uani 1 1 d . . .
N1 N 0.6418(3) 0.40942(11) 0.35815(6) 0.0411(3) Uani 1 1 d . . .
C2 C 0.5225(3) 0.38135(13) 0.42167(7) 0.0393(3) Uani 1 1 d . . .
C6 C 0.5327(3) 0.50670(13) 0.31309(8) 0.0409(3) Uani 1 1 d . . .
N3 N 0.3016(3) 0.44941(11) 0.44181(6) 0.0413(3) Uani 1 1 d . . .
C15 C 0.6026(5) 0.7066(2) -0.03182(10) 0.0649(5) Uani 1 1 d . . .
C14 C 0.7141(5) 0.96546(18) 0.08318(11) 0.0605(5) Uani 1 1 d . . .
C5 C 0.3140(3) 0.58051(13) 0.32969(7) 0.0384(3) Uani 1 1 d . . .
O1 O 0.5817(3) 0.88551(10) 0.05508(6) 0.0573(3) Uani 1 1 d . . .
C4 C 0.2000(3) 0.54807(12) 0.39827(7) 0.0375(3) Uani 1 1 d . . .
C10 C 0.4456(3) 0.79842(13) 0.09816(8) 0.0419(4) Uani 1 1 d . . .
C9 C 0.4121(3) 0.78635(13) 0.16798(8) 0.0422(4) Uani 1 1 d . . .
C11 C 0.3266(3) 0.72107(13) 0.06766(7) 0.0401(3) Uani 1 1 d . . .
O2 O 0.3316(2) 0.73796(10) -0.00166(5) 0.0478(3) Uani 1 1 d . . .
C8 C 0.2596(3) 0.69715(13) 0.20721(7) 0.0407(3) Uani 1 1 d . . .
C7 C 0.1944(4) 0.69136(15) 0.28168(8) 0.0464(4) Uani 1 1 d . . .
C12 C 0.1849(3) 0.62775(13) 0.10797(8) 0.0407(3) Uani 1 1 d . . .
C13 C 0.1512(3) 0.61612(14) 0.17740(8) 0.0432(4) Uani 1 1 d . . .
N4 N -0.0149(3) 0.61435(13) 0.42046(7) 0.0478(4) Uani 1 1 d . . .
O3 O 0.0881(3) 0.55259(10) 0.07427(6) 0.0520(3) Uani 1 1 d . . .
C16 C -0.0869(5) 0.46483(17) 0.11147(12) 0.0590(5) Uani 1 1 d . . .
C23 C 1.8939(4) 0.04517(17) 0.22835(10) 0.0551(4) Uani 1 1 d . . .
C24 C 1.7831(4) -0.02268(16) 0.28731(10) 0.0550(4) Uani 1 1 d . . .
O4 O 1.5661(4) -0.17564(12) 0.39406(8) 0.0774(5) Uani 1 1 d . . .
C22 C 1.7741(4) 0.15816(17) 0.20475(10) 0.0551(4) Uani 1 1 d . . .
C17 C 1.4612(4) -0.07355(16) 0.38714(10) 0.0589(5) Uani 1 1 d . . .
C19 C 1.5528(3) 0.01902(14) 0.32524(8) 0.0452(4) Uani 1 1 d . . .
C21 C 1.5485(4) 0.20274(15) 0.24149(10) 0.0502(4) Uani 1 1 d . . .
O5 O 1.2761(4) -0.04533(14) 0.43118(8) 0.0900(6) Uani 1 1 d . . .
C20 C 1.4351(3) 0.13694(13) 0.30189(8) 0.0419(4) Uani 1 1 d . . .
C18 C 1.1910(3) 0.20335(14) 0.33514(9) 0.0473(4) Uani 1 1 d . . .
O6 O 1.0863(3) 0.15683(13) 0.39302(7) 0.0724(4) Uani 1 1 d . . .
O7 O 1.1035(3) 0.30345(10) 0.30354(7) 0.0616(4) Uani 1 1 d . . .
H1 H 0.491(4) 0.8403(17) 0.1879(10) 0.054(5) Uiso 1 1 d . . .
H2 H 0.629(4) 0.5221(15) 0.2678(9) 0.045(4) Uiso 1 1 d . . .
H3 H -0.081(4) 0.6848(18) 0.3945(10) 0.050(5) Uiso 1 1 d . . .
H4 H 0.057(4) 0.5502(17) 0.2039(9) 0.048(5) Uiso 1 1 d . . .
H5 H 1.464(5) 0.2862(19) 0.2270(10) 0.062(5) Uiso 1 1 d . . .
H6 H 0.763(5) 0.2339(19) 0.4486(11) 0.059(5) Uiso 1 1 d . . .
H7 H 0.261(4) 0.7612(17) 0.2930(9) 0.050(5) Uiso 1 1 d . . .
H8 H 1.874(4) -0.1023(19) 0.3055(10) 0.062(6) Uiso 1 1 d . . .
H9 H -0.081(5) 0.5939(18) 0.4627(12) 0.060(5) Uiso 1 1 d . . .
H10 H 0.560(5) 0.255(2) 0.5089(13) 0.075(7) Uiso 1 1 d . . .
H11 H 0.803(5) 0.3614(18) 0.3461(10) 0.061(5) Uiso 1 1 d . . .
H12 H 2.055(5) 0.012(2) 0.2040(12) 0.075(6) Uiso 1 1 d . . .
H13 H -0.023(4) 0.7017(17) 0.2886(10) 0.055(5) Uiso 1 1 d . . .
H14 H -0.264(6) 0.502(2) 0.1315(12) 0.080(7) Uiso 1 1 d . . .
H15 H 1.844(5) 0.205(2) 0.1606(13) 0.078(7) Uiso 1 1 d . . .
H16 H 1.192(7) 0.044(3) 0.4177(15) 0.109(9) Uiso 1 1 d . . .
H17 H 0.015(5) 0.417(2) 0.1482(12) 0.076(7) Uiso 1 1 d . . .
H18 H 0.855(5) 0.919(2) 0.1186(12) 0.072(6) Uiso 1 1 d . . .
H19 H 0.572(5) 1.0052(19) 0.1067(11) 0.067(6) Uiso 1 1 d . . .
H20 H -0.146(5) 0.425(2) 0.0755(12) 0.071(6) Uiso 1 1 d . . .
H21 H 0.812(5) 1.020(2) 0.0442(13) 0.078(7) Uiso 1 1 d . . .
H22 H 0.598(6) 0.713(2) -0.0789(15) 0.092(8) Uiso 1 1 d . . .
H23 H 0.660(6) 0.613(3) -0.0175(15) 0.105(9) Uiso 1 1 d . . .
H25 H 0.765(7) 0.736(2) -0.0153(15) 0.103(9) Uiso 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
N2 C2 1.316(2) . ?
N1 C2 1.353(2) . ?
N1 C6 1.356(2) . ?
C2 N3 1.3372(19) . ?
C6 C5 1.344(2) . ?
N3 C4 1.3399(19) . ?
C15 O2 1.418(2) . ?
C14 O1 1.415(2) . ?
C5 C4 1.437(2) . ?
C5 C7 1.505(2) . ?
O1 C10 1.3576(19) . ?
C4 N4 1.3235(19) . ?
C10 C11 1.389(2) . ?
C10 C9 1.395(2) . ?
C9 C8 1.383(2) . ?
C11 O2 1.3769(18) . ?
C11 C12 1.397(2) . ?
C8 C13 1.391(2) . ?
C8 C7 1.513(2) . ?
C12 O3 1.363(2) . ?
C12 C13 1.388(2) . ?
O3 C16 1.419(2) . ?
C23 C22 1.367(3) . ?
C23 C24 1.374(3) . ?
C24 C19 1.394(2) . ?
O4 C17 1.222(2) . ?
C22 C21 1.379(3) . ?
C17 O5 1.278(2) . ?
C17 C19 1.522(3) . ?
C19 C20 1.412(2) . ?
C21 C20 1.390(2) . ?
C20 C18 1.522(2) . ?
C18 O7 1.236(2) . ?
C18 O6 1.263(2) . ?
 
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
C2 N1 C6 119.90(13) . . ?
N2 C2 N3 120.94(14) . . ?
N2 C2 N1 117.77(14) . . ?
N3 C2 N1 121.29(14) . . ?
C5 C6 N1 122.38(14) . . ?
C2 N3 C4 119.05(13) . . ?
C6 C5 C4 115.37(14) . . ?
C6 C5 C7 123.78(14) . . ?
C4 C5 C7 120.84(13) . . ?
C10 O1 C14 117.92(14) . . ?
N4 C4 N3 117.29(13) . . ?
N4 C4 C5 120.76(14) . . ?
N3 C4 C5 121.94(13) . . ?
O1 C10 C11 115.16(14) . . ?
O1 C10 C9 124.51(15) . . ?
C11 C10 C9 120.29(14) . . ?
C8 C9 C10 120.06(15) . . ?
O2 C11 C10 121.42(14) . . ?
O2 C11 C12 119.17(14) . . ?
C10 C11 C12 119.32(14) . . ?
C11 O2 C15 115.02(13) . . ?
C9 C8 C13 119.90(14) . . ?
C9 C8 C7 120.37(15) . . ?
C13 C8 C7 119.63(15) . . ?
C5 C7 C8 115.77(12) . . ?
O3 C12 C13 124.38(14) . . ?
O3 C12 C11 115.42(13) . . ?
C13 C12 C11 120.20(15) . . ?
C12 C13 C8 120.09(15) . . ?
C12 O3 C16 117.60(14) . . ?
C22 C23 C24 119.44(17) . . ?
C23 C24 C19 122.78(16) . . ?
C23 C22 C21 119.28(18) . . ?
O4 C17 O5 120.29(18) . . ?
O4 C17 C19 119.04(17) . . ?
O5 C17 C19 120.67(15) . . ?
C24 C19 C20 117.70(16) . . ?
C24 C19 C17 113.22(15) . . ?
C20 C19 C17 129.07(15) . . ?
C22 C21 C20 122.60(16) . . ?
C21 C20 C19 118.16(15) . . ?
C21 C20 C18 114.28(14) . . ?
C19 C20 C18 127.56(15) . . ?
O7 C18 O6 122.20(15) . . ?
O7 C18 C20 117.38(16) . . ?
O6 C18 C20 120.42(15) . . ?
 
_diffrn_measured_fraction_theta_max    0.991
_diffrn_reflns_theta_full              67.10
_diffrn_measured_fraction_theta_full   0.991
_refine_diff_density_max    0.258
_refine_diff_density_min   -0.234
_refine_diff_density_rms    0.070
 

===============================================================================

data_compound 2 (Trimethoprim hydrogen adipate)
 

_publ_contact_author
;
Packianathan Thomas Muthiah
Department of Chemistry,
Bharathidasan University,
Tiruchirappalli-640 024
India.
;
_publ_contact_author_phone        '91-431-2407053'
_publ_contact_author_fax         
_publ_contact_author_email        'tommtrichy@yahoo.co.in'

loop_
 _publ_author_name
 _publ_author_address
 'Savarimuthu Francis'
;
Department of Chemistry,
Bharathidasan University,
Tiruchirappalli-620 024
India
;

 'Packianathan Thomas Muthiah'
;
Department of Chemistry,
Bharathidasan University,
Tiruchirappalli-620 024
India
;
 'Rychlewska, Urszula'
;
Department of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Poznań
Poland
;
 'Warżajtis, Beata'
;
Department of Chemistry
Adam Mickiewicz University
Grunwaldzka 6
60-780 Poznań
Poland
;
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C20 H28 N4 O7'
_chemical_formula_weight          436.46
 
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'
 
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    'P -1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    8.172(2)
_cell_length_b                    9.4744(8)
_cell_length_c                    13.8162(8)
_cell_angle_alpha                 85.741(6)
_cell_angle_beta                  87.430(10)
_cell_angle_gamma                 88.680(10)
_cell_volume                      1065.5(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     294(2)
_cell_measurement_reflns_used     76
_cell_measurement_theta_min       6.41
_cell_measurement_theta_max       24.95
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.50
_exptl_crystal_size_mid           0.30
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.360
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              464
_exptl_absorpt_coefficient_mu     0.870
_exptl_absorpt_correction_type    'none'
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       294(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   ' KM-4 four circle diffractometer'
_diffrn_measurement_method        ' Θ--2Θ'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          2
_diffrn_standards_interval_count  100
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0.04
_diffrn_reflns_number             3706
_diffrn_reflns_av_R_equivalents   0.0211
_diffrn_reflns_av_sigmaI/netI     0.0151
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          3.21
_diffrn_reflns_theta_max          67.07
_reflns_number_total              3637
_reflns_number_gt                 3062
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'Kuma KM-4 software (Kuma Diffraction, 1991)
_computing_cell_refinement        'Kuma KM-4 software (Kuma Diffraction, 1991)
_computing_data_reduction         'Kuma KM-4 software (Kuma Diffraction, 1991)
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)'
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0847P)²+0.2134P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0049(9)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          3637
_refine_ls_number_parameters      404
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0531
_refine_ls_R_factor_gt            0.0439
_refine_ls_wR_factor_ref          0.1334
_refine_ls_wR_factor_gt           0.1270
_refine_ls_goodness_of_fit_ref    1.043
_refine_ls_restrained_S_all       1.043
_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_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C2 C 0.6359(2) 0.52797(18) 0.09667(11) 0.0436(4) Uani 1 1 d . . .
C4 C 0.4020(2) 0.46610(18) 0.18502(12) 0.0446(4) Uani 1 1 d . . .
C5 C 0.3213(2) 0.59689(18) 0.15471(11) 0.0439(4) Uani 1 1 d . . .
C6 C 0.4119(2) 0.6871(2) 0.09572(12) 0.0485(4) Uani 1 1 d . . .
H6 H 0.370(3) 0.774(2) 0.0672(15) 0.056(5) Uiso 1 1 d . . .
C7 C 0.1422(2) 0.6236(2) 0.17668(13) 0.0529(5) Uani 1 1 d . . .
H71 H 0.076(3) 0.547(2) 0.1527(16) 0.063(6) Uiso 1 1 d . . .
H72 H 0.112(3) 0.708(3) 0.1355(18) 0.073(7) Uiso 1 1 d . . .
C8 C 0.0892(2) 0.63947(18) 0.28194(12) 0.0439(4) Uani 1 1 d . . .
C9 C 0.1862(2) 0.70661(19) 0.34385(13) 0.0460(4) Uani 1 1 d . . .
H9 H 0.287(3) 0.737(2) 0.3217(15) 0.055(5) Uiso 1 1 d . . .
C10 C 0.1276(2) 0.72816(17) 0.43762(12) 0.0439(4) Uani 1 1 d . . .
C11 C -0.0295(2) 0.68510(17) 0.46925(11) 0.0427(4) Uani 1 1 d . . .
C12 C -0.1243(2) 0.61594(17) 0.40732(12) 0.0433(4) Uani 1 1 d . . .
C13 C -0.0642(2) 0.59223(19) 0.31416(12) 0.0465(4) Uani 1 1 d . . .
H13 H -0.130(3) 0.547(2) 0.2722(15) 0.056(5) Uiso 1 1 d . . .
C14 C 0.3773(3) 0.8298(3) 0.47887(18) 0.0601(5) Uani 1 1 d . . .
H141 H 0.441(3) 0.747(2) 0.4627(16) 0.062(6) Uiso 1 1 d . . .
H142 H 0.416(3) 0.865(3) 0.5390(19) 0.079(7) Uiso 1 1 d . . .
H143 H 0.382(3) 0.901(3) 0.4198(19) 0.079(7) Uiso 1 1 d . . .
C15 C -0.1663(3) 0.8469(2) 0.56254(16) 0.0623(5) Uani 1 1 d . . .
H151 H -0.083(4) 0.920(4) 0.545(2) 0.110(10) Uiso 1 1 d . . .
H152 H -0.201(3) 0.858(2) 0.6283(18) 0.072(7) Uiso 1 1 d . . .
H153 H -0.264(4) 0.850(3) 0.520(3) 0.117(11) Uiso 1 1 d . . .
C16 C -0.3764(3) 0.5078(3) 0.38070(16) 0.0597(5) Uani 1 1 d . . .
H161 H -0.395(3) 0.577(3) 0.3201(17) 0.071(6) Uiso 1 1 d . . .
H162 H -0.479(3) 0.494(2) 0.4167(18) 0.073(7) Uiso 1 1 d . . .
H163 H -0.322(3) 0.421(3) 0.3613(18) 0.078(7) Uiso 1 1 d . . .
O1 O 0.21226(15) 0.79317(14) 0.50413(9) 0.0548(3) Uani 1 1 d . . .
O2 O -0.08946(15) 0.71101(13) 0.56100(8) 0.0506(3) Uani 1 1 d . . .
O3 O -0.27656(15) 0.57634(14) 0.44383(9) 0.0545(3) Uani 1 1 d . . .
N1 N 0.56988(18) 0.65561(16) 0.06845(10) 0.0487(4) Uani 1 1 d . . .
N3 N 0.55463(17) 0.43233(15) 0.15367(10) 0.0470(4) Uani 1 1 d . . .
N2 N 0.78902(19) 0.5010(2) 0.06559(12) 0.0541(4) Uani 1 1 d . . .
H21 H 0.844(3) 0.567(2) 0.0288(16) 0.060(6) Uiso 1 1 d . . .
H22 H 0.838(3) 0.415(3) 0.0822(18) 0.073(7) Uiso 1 1 d . . .
N4 N 0.3265(2) 0.37063(19) 0.24557(13) 0.0592(4) Uani 1 1 d . . .
H41 H 0.235(3) 0.395(2) 0.2750(17) 0.065(6) Uiso 1 1 d . . .
H42 H 0.373(3) 0.287(3) 0.2622(19) 0.080(8) Uiso 1 1 d . . .
C17 C 0.8805(2) 0.8148(2) -0.08393(14) 0.0554(5) Uani 1 1 d . . .
C18 C 0.9630(4) 0.9327(4) -0.1483(3) 0.0622(8) Uani 0.77 1 d P . .
H181 H 0.876(4) 0.986(3) -0.186(2) 0.108(10) Uiso 1 1 d . . .
H182 H 1.012(4) 0.999(4) -0.107(2) 0.075(9) Uiso 0.77 1 d P . .
C18A C 0.9450(18) 0.8924(16) -0.1751(10) 0.068(4) Uiso 0.23 1 d P . .
H18A H 0.9429 0.8305 -0.2269 0.08(3) Uiso 0.23 1 d PR . .
C19 C 1.0969(3) 0.8762(3) -0.21924(19) 0.0545(6) Uani 0.77 1 d P . .
H191 H 1.186(3) 0.824(3) -0.1873(18) 0.048(6) Uiso 0.77 1 d P . .
H192 H 1.052(4) 0.806(3) -0.260(2) 0.075(9) Uiso 0.77 1 d P . .
C19A C 1.1086(12) 0.9430(11) -0.1683(7) 0.062(2) Uiso 0.23 1 d P . .
H19A H 1.1773 0.8669 -0.1426 0.05(2) Uiso 0.23 1 d PR . .
H19B H 1.1088 1.0184 -0.1256 0.09(4) Uiso 0.23 1 d PR . .
C20 C 1.1774(3) 0.9986(3) -0.28095(18) 0.0711(6) Uani 1 1 d . . .
H201 H 1.087(3) 1.076(3) -0.3033(18) 0.079(7) Uiso 1 1 d . . .
H202 H 1.235(4) 0.947(4) -0.340(3) 0.127(11) Uiso 1 1 d . . .
C21 C 1.3076(3) 1.0784(3) -0.2364(2) 0.0726(6) Uani 1 1 d . . .
H211 H 1.349(3) 1.146(3) -0.276(2) 0.084(8) Uiso 1 1 d . . .
H212 H 1.236(4) 1.106(3) -0.175(2) 0.095(8) Uiso 1 1 d . . .
C22 C 1.4565(2) 0.98764(19) -0.21235(16) 0.0576(5) Uani 1 1 d . . .
O5 O 0.96097(17) 0.71001(17) -0.05430(12) 0.0750(5) Uani 1 1 d . . .
O4 O 0.73297(16) 0.83696(16) -0.05713(11) 0.0664(4) Uani 1 1 d . . .
H5O H 0.634(3) 0.719(2) 0.0256(16) 0.065(6) Uiso 1 1 d . . .
O6 O 1.5286(2) 0.91728(18) -0.27051(12) 0.0776(5) Uani 1 1 d . . .
O7 O 1.4978(2) 0.99283(17) -0.12295(13) 0.0764(5) Uani 1 1 d . . .
H7O H 1.591(5) 0.943(4) -0.105(2) 0.115(11) Uiso 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C2 N3 1.326(2) . ?
C2 N2 1.330(2) . ?
C2 N1 1.351(2) . ?
C4 N4 1.329(2) . ?
C4 N3 1.341(2) . ?
C4 C5 1.434(2) . ?
C5 C6 1.347(3) . ?
C5 C7 1.501(2) . ?
C6 N1 1.361(2) . ?
C6 H6 0.95(2) . ?
C7 C8 1.516(2) . ?
C7 H71 1.00(2) . ?
C7 H72 0.98(3) . ?
C8 C13 1.384(3) . ?
C8 C9 1.389(2) . ?
C9 C10 1.389(2) . ?
C9 H9 0.91(2) . ?
C10 O1 1.365(2) . ?
C10 C11 1.398(2) . ?
C11 O2 1.3756(19) . ?
C11 C12 1.389(2) . ?
C12 O3 1.371(2) . ?
C12 C13 1.389(2) . ?
C13 H13 0.94(2) . ?
C14 O1 1.422(2) . ?
C14 H141 0.96(2) . ?
C14 H142 0.99(3) . ?
C14 H143 1.02(3) . ?
C15 O2 1.421(2) . ?
C15 H151 0.99(3) . ?
C15 H152 0.95(2) . ?
C15 H153 1.02(4) . ?
C16 O3 1.421(2) . ?
C16 H161 1.04(2) . ?
C16 H162 0.96(3) . ?
C16 H163 0.98(3) . ?
N1 H5O 0.96(2) . ?
N2 H21 0.90(2) . ?
N2 H22 0.92(3) . ?
N4 H41 0.87(3) . ?
N4 H42 0.89(3) . ?
C17 O5 1.233(2) . ?
C17 O4 1.263(2) . ?
C17 C18A 1.492(15) . ?
C17 C18 1.525(4) . ?
C18 C18A 0.577(13) . ?
C18 C19A 1.214(10) . ?
C18 C19 1.549(4) . ?
C18 H181 1.00(4) . ?
C18 H182 0.98(3) . ?
C18 H18A 1.5247 . ?
C18 H19B 1.5146 . ?
C18A C19 1.369(15) . ?
C18A C19A 1.439(17) . ?
C18A H181 1.04(4) . ?
C18A H182 1.55(3) . ?
C18A H18A 0.9599 . ?
C19 C19A 0.990(10) . ?
C19 C20 1.531(3) . ?
C19 H18A 1.3512 . ?
C19 H191 0.97(3) . ?
C19 H192 0.99(3) . ?
C19 H19A 1.2676 . ?
C19A C20 1.682(10) . ?
C19A H182 1.27(3) . ?
C19A H191 1.32(3) . ?
C19A H19A 0.9600 . ?
C19A H19B 0.9600 . ?
C20 C21 1.498(4) . ?
C20 H201 1.07(3) . ?
C20 H202 1.07(4) . ?
C21 C22 1.509(3) . ?
C21 H211 0.88(3) . ?
C21 H212 1.05(3) . ?
C22 O6 1.207(2) . ?
C22 O7 1.300(3) . ?
O7 H7O 0.92(4) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N3 C2 N2 120.29(17) . . ?
N3 C2 N1 122.51(15) . . ?
N2 C2 N1 117.19(16) . . ?
N4 C4 N3 116.52(17) . . ?
N4 C4 C5 120.81(16) . . ?
N3 C4 C5 122.66(16) . . ?
C6 C5 C4 115.40(16) . . ?
C6 C5 C7 122.01(17) . . ?
C4 C5 C7 122.15(16) . . ?
C5 C6 N1 121.67(17) . . ?
C5 C6 H6 123.5(13) . . ?
N1 C6 H6 114.8(13) . . ?
C5 C7 C8 117.06(15) . . ?
C5 C7 H71 110.0(13) . . ?
C8 C7 H71 107.9(13) . . ?
C5 C7 H72 106.2(14) . . ?
C8 C7 H72 111.1(14) . . ?
H71 C7 H72 103.8(18) . . ?
C13 C8 C9 120.10(16) . . ?
C13 C8 C7 118.13(16) . . ?
C9 C8 C7 121.67(16) . . ?
C10 C9 C8 119.73(16) . . ?
C10 C9 H9 121.0(13) . . ?
C8 C9 H9 119.3(13) . . ?
O1 C10 C9 124.56(16) . . ?
O1 C10 C11 115.12(14) . . ?
C9 C10 C11 120.30(15) . . ?
O2 C11 C12 120.36(15) . . ?
O2 C11 C10 120.20(15) . . ?
C12 C11 C10 119.44(15) . . ?
O3 C12 C11 115.95(14) . . ?
O3 C12 C13 123.96(16) . . ?
C11 C12 C13 120.08(16) . . ?
C8 C13 C12 120.28(16) . . ?
C8 C13 H13 120.0(12) . . ?
C12 C13 H13 119.7(13) . . ?
O1 C14 H141 110.6(13) . . ?
O1 C14 H142 103.3(15) . . ?
H141 C14 H142 110(2) . . ?
O1 C14 H143 110.3(14) . . ?
H141 C14 H143 107.7(19) . . ?
H142 C14 H143 115(2) . . ?
O2 C15 H151 108.7(19) . . ?
O2 C15 H152 106.5(15) . . ?
H151 C15 H152 107(2) . . ?
O2 C15 H153 108.5(19) . . ?
H151 C15 H153 115(3) . . ?
H152 C15 H153 110(2) . . ?
O3 C16 H161 107.9(13) . . ?
O3 C16 H162 104.9(14) . . ?
H161 C16 H162 109.1(19) . . ?
O3 C16 H163 109.8(15) . . ?
H161 C16 H163 110.1(19) . . ?
H162 C16 H163 115(2) . . ?
C10 O1 C14 117.71(14) . . ?
C11 O2 C15 111.55(13) . . ?
C12 O3 C16 116.66(14) . . ?
C2 N1 C6 119.64(16) . . ?
C2 N1 H5O 118.4(14) . . ?
C6 N1 H5O 121.8(14) . . ?
C2 N3 C4 117.94(15) . . ?
C2 N2 H21 119.9(14) . . ?
C2 N2 H22 120.0(15) . . ?
H21 N2 H22 120(2) . . ?
C4 N4 H41 118.5(15) . . ?
C4 N4 H42 121.7(17) . . ?
H41 N4 H42 119(2) . . ?
O5 C17 O4 123.12(18) . . ?
O5 C17 C18A 116.2(6) . . ?
O4 C17 C18A 118.1(6) . . ?
O5 C17 C18 120.09(19) . . ?
O4 C17 C18 116.52(19) . . ?
C18A C17 C18 22.0(5) . . ?
C18A C18 C19A 100.9(17) . . ?
C18A C18 C17 75.8(16) . . ?
C19A C18 C17 126.6(5) . . ?
C18A C18 C19 61.3(16) . . ?
C19A C18 C19 39.7(5) . . ?
C17 C18 C19 112.7(3) . . ?
C18A C18 H181 78(2) . . ?
C19A C18 H181 123.6(18) . . ?
C17 C18 H181 107.9(18) . . ?
C19 C18 H181 109.9(19) . . ?
C18A C18 H182 171(3) . . ?
C19A C18 H182 70(2) . . ?
C17 C18 H182 109(2) . . ?
C19 C18 H182 109(2) . . ?
H181 C18 H182 108(3) . . ?
C18A C18 H18A 9.3 . . ?
C19A C18 H18A 91.8 . . ?
C17 C18 H18A 82.7 . . ?
C19 C18 H18A 52.1 . . ?
H181 C18 H18A 81.0 . . ?
H182 C18 H18A 161.4 . . ?
C18A C18 H19B 139.8 . . ?
C19A C18 H19B 39.3 . . ?
C17 C18 H19B 127.6 . . ?
C19 C18 H19B 78.7 . . ?
H181 C18 H19B 115.6 . . ?
H182 C18 H19B 31.0 . . ?
H18A C18 H19B 130.5 . . ?
C18 C18A C19 97.1(18) . . ?
C18 C18A C19A 55.9(14) . . ?
C19 C18A C19A 41.2(6) . . ?
C18 C18A C17 82.2(16) . . ?
C19 C18A C17 126.9(11) . . ?
C19A C18A C17 113.5(10) . . ?
C18 C18A H181 70(2) . . ?
C19 C18A H181 122(2) . . ?
C19A C18A H181 103(2) . . ?
C17 C18A H181 108(2) . . ?
C18 C18A H182 5.9(16) . . ?
C19 C18A H182 91.1(16) . . ?
C19A C18A H182 50.0(14) . . ?
C17 C18A H182 85.5(15) . . ?
H181 C18A H182 73(2) . . ?
C18 C18A H18A 165.1 . . ?
C19 C18A H18A 68.4 . . ?
C19A C18A H18A 109.5 . . ?
C17 C18A H18A 108.5 . . ?
H181 C18A H18A 114.9 . . ?
H182 C18A H18A 159.3 . . ?
C19A C19 C18A 73.3(8) . . ?
C19A C19 C20 80.6(6) . . ?
C18A C19 C20 121.1(7) . . ?
C19A C19 C18 51.6(6) . . ?
C18A C19 C18 21.7(5) . . ?
C20 C19 C18 110.6(2) . . ?
C19A C19 H18A 114.6 . . ?
C18A C19 H18A 41.3 . . ?
C20 C19 H18A 126.0 . . ?
C18 C19 H18A 63.0 . . ?
C19A C19 H191 84.3(16) . . ?
C18A C19 H191 122.3(16) . . ?
C20 C19 H191 105.9(15) . . ?
C18 C19 H191 114.0(15) . . ?
H18A C19 H191 126.2 . . ?
C19A C19 H192 163(2) . . ?
C18A C19 H192 89(2) . . ?
C20 C19 H192 111.4(18) . . ?
C18 C19 H192 111.2(19) . . ?
H18A C19 H192 48.3 . . ?
H191 C19 H192 103(2) . . ?
C19A C19 H19A 48.4 . . ?
C18A C19 H19A 97.0 . . ?
C20 C19 H19A 103.5 . . ?
C18 C19 H19A 81.3 . . ?
H18A C19 H19A 125.8 . . ?
H191 C19 H19A 37.1 . . ?
H192 C19 H19A 134.4 . . ?
C19 C19A C18 88.7(8) . . ?
C19 C19A C18A 65.6(8) . . ?
C18 C19A C18A 23.2(6) . . ?
C19 C19A C20 63.9(5) . . ?
C18 C19A C20 121.1(7) . . ?
C18A C19A C20 107.8(8) . . ?
C19 C19A H182 135.2(19) . . ?
C18 C19A H182 46.5(16) . . ?
C18A C19A H182 69.7(17) . . ?
C20 C19A H182 132.3(17) . . ?
C19 C19A H191 47.3(12) . . ?
C18 C19A H191 115.2(14) . . ?
C18A C19A H191 96.6(14) . . ?
C20 C19A H191 84.1(12) . . ?
H182 C19A H191 143(2) . . ?
C19 C19A H19A 81.1 . . ?
C18 C19A H19A 115.9 . . ?
C18A C19A H19A 109.2 . . ?
C20 C19A H19A 110.0 . . ?
H182 C19A H19A 115.7 . . ?
H191 C19A H19A 35.0 . . ?
C19 C19A H19B 170.4 . . ?
C18 C19A H19B 87.5 . . ?
C18A C19A H19B 110.5 . . ?
C20 C19A H19B 110.9 . . ?
H182 C19A H19B 41.6 . . ?
H191 C19A H19B 142.0 . . ?
H19A C19A H19B 108.5 . . ?
C21 C20 C19 117.9(2) . . ?
C21 C20 C19A 88.6(4) . . ?
C19 C20 C19A 35.5(3) . . ?
C21 C20 H201 105.9(13) . . ?
C19 C20 H201 110.0(13) . . ?
C19A C20 H201 102.7(14) . . ?
C21 C20 H202 107.0(18) . . ?
C19 C20 H202 102.8(18) . . ?
C19A C20 H202 133.9(19) . . ?
H201 C20 H202 113(2) . . ?
C20 C21 C22 112.9(2) . . ?
C20 C21 H211 112.8(18) . . ?
C22 C21 H211 102.4(18) . . ?
C20 C21 H212 96.4(16) . . ?
C22 C21 H212 113.9(16) . . ?
H211 C21 H212 119(2) . . ?
O6 C22 O7 123.88(19) . . ?
O6 C22 C21 123.1(2) . . ?
O7 C22 C21 113.1(2) . . ?
C22 O7 H7O 117(2) . . ?
 
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
N4 C4 C5 C6 177.99(16) . . . . ?
N3 C4 C5 C6 -2.9(2) . . . . ?
N4 C4 C5 C7 -9.5(2) . . . . ?
N3 C4 C5 C7 169.63(15) . . . . ?
C4 C5 C6 N1 -0.9(2) . . . . ?
C7 C5 C6 N1 -173.39(15) . . . . ?
C6 C5 C7 C8 -118.8(2) . . . . ?
C4 C5 C7 C8 69.1(2) . . . . ?
C5 C7 C8 C13 -147.13(17) . . . . ?
C5 C7 C8 C9 36.5(3) . . . . ?
C13 C8 C9 C10 -1.0(3) . . . . ?
C7 C8 C9 C10 175.20(16) . . . . ?
C8 C9 C10 O1 -179.78(15) . . . . ?
C8 C9 C10 C11 -1.2(3) . . . . ?
O1 C10 C11 O2 1.0(2) . . . . ?
C9 C10 C11 O2 -177.72(14) . . . . ?
O1 C10 C11 C12 -178.99(14) . . . . ?
C9 C10 C11 C12 2.3(2) . . . . ?
O2 C11 C12 O3 -0.3(2) . . . . ?
C10 C11 C12 O3 179.62(14) . . . . ?
O2 C11 C12 C13 178.90(15) . . . . ?
C10 C11 C12 C13 -1.1(2) . . . . ?
C9 C8 C13 C12 2.2(3) . . . . ?
C7 C8 C13 C12 -174.14(16) . . . . ?
O3 C12 C13 C8 178.04(15) . . . . ?
C11 C12 C13 C8 -1.1(3) . . . . ?
C9 C10 O1 C14 -6.0(3) . . . . ?
C11 C10 O1 C14 175.36(16) . . . . ?
C12 C11 O2 C15 -93.0(2) . . . . ?
C10 C11 O2 C15 87.1(2) . . . . ?
C11 C12 O3 C16 178.83(16) . . . . ?
C13 C12 O3 C16 -0.4(3) . . . . ?
N3 C2 N1 C6 -2.6(2) . . . . ?
N2 C2 N1 C6 178.01(15) . . . . ?
C5 C6 N1 C2 3.5(2) . . . . ?
N2 C2 N3 C4 178.34(15) . . . . ?
N1 C2 N3 C4 -1.0(2) . . . . ?
N4 C4 N3 C2 -177.03(15) . . . . ?
C5 C4 N3 C2 3.8(2) . . . . ?
O5 C17 C18 C18A 85.9(17) . . . . ?
O4 C17 C18 C18A -99.9(17) . . . . ?
O5 C17 C18 C19A -7.3(9) . . . . ?
O4 C17 C18 C19A 166.9(7) . . . . ?
C18A C17 C18 C19A -93.2(18) . . . . ?
O5 C17 C18 C19 36.0(4) . . . . ?
O4 C17 C18 C19 -149.8(3) . . . . ?
C18A C17 C18 C19 -49.9(16) . . . . ?
C19A C18 C18A C19 -1.1(13) . . . . ?
C17 C18 C18A C19 -126.4(11) . . . . ?
C17 C18 C18A C19A -125.3(6) . . . . ?
C19 C18 C18A C19A 1.1(13) . . . . ?
C19A C18 C18A C17 125.3(6) . . . . ?
C19 C18 C18A C17 126.4(11) . . . . ?
O5 C17 C18A C18 -105.9(16) . . . . ?
O4 C17 C18A C18 91.6(16) . . . . ?
O5 C17 C18A C19 -12.9(14) . . . . ?
O4 C17 C18A C19 -175.4(9) . . . . ?
C18 C17 C18A C19 93(2) . . . . ?
O5 C17 C18A C19A -58.4(12) . . . . ?
O4 C17 C18A C19A 139.0(9) . . . . ?
C18 C17 C18A C19A 47.5(12) . . . . ?
C18 C18A C19 C19A 1.4(16) . . . . ?
C17 C18A C19 C19A -84.1(13) . . . . ?
C18 C18A C19 C20 -66.3(19) . . . . ?
C19A C18A C19 C20 -67.7(8) . . . . ?
C17 C18A C19 C20 -151.8(9) . . . . ?
C19A C18A C19 C18 -1.4(16) . . . . ?
C17 C18A C19 C18 -85.5(19) . . . . ?
C18A C18 C19 C19A -178(2) . . . . ?
C17 C18 C19 C19A -120.5(8) . . . . ?
C19A C18 C19 C18A 178(2) . . . . ?
C17 C18 C19 C18A 57.7(18) . . . . ?
C18A C18 C19 C20 123.1(18) . . . . ?
C19A C18 C19 C20 -58.6(7) . . . . ?
C17 C18 C19 C20 -179.2(3) . . . . ?
C18A C19 C19A C18 -0.7(8) . . . . ?
C20 C19 C19A C18 125.9(5) . . . . ?
C20 C19 C19A C18A 126.6(7) . . . . ?
C18 C19 C19A C18A 0.7(8) . . . . ?
C18A C19 C19A C20 -126.6(7) . . . . ?
C18 C19 C19A C20 -125.9(5) . . . . ?
C18A C18 C19A C19 1.5(18) . . . . ?
C17 C18 C19A C19 81.9(8) . . . . ?
C17 C18 C19A C18A 80.3(17) . . . . ?
C19 C18 C19A C18A -1.5(18) . . . . ?
C18A C18 C19A C20 59.7(19) . . . . ?
C17 C18 C19A C20 140.0(6) . . . . ?
C19 C18 C19A C20 58.2(7) . . . . ?
C18 C18A C19A C19 -178(2) . . . . ?
C17 C18A C19A C19 119.9(11) . . . . ?
C19 C18A C19A C18 178(2) . . . . ?
C17 C18A C19A C18 -61.8(14) . . . . ?
C18 C18A C19A C20 -129.1(16) . . . . ?
C19 C18A C19A C20 49.2(6) . . . . ?
C17 C18A C19A C20 169.1(8) . . . . ?
C19A C19 C20 C21 37.8(6) . . . . ?
C18A C19 C20 C21 101.7(7) . . . . ?
C18 C19 C20 C21 80.5(3) . . . . ?
C18A C19 C20 C19A 63.9(9) . . . . ?
C18 C19 C20 C19A 42.7(6) . . . . ?
C19 C19A C20 C21 -147.2(5) . . . . ?
C18 C19A C20 C21 141.7(8) . . . . ?
C18A C19A C20 C21 162.6(8) . . . . ?
C18 C19A C20 C19 -71.1(8) . . . . ?
C18A C19A C20 C19 -50.2(8) . . . . ?
C19 C20 C21 C22 63.7(3) . . . . ?
C19A C20 C21 C22 84.5(4) . . . . ?
C20 C21 C22 O6 52.1(3) . . . . ?
C20 C21 C22 O7 -127.6(2) . . . . ?
 
_diffrn_measured_fraction_theta_max    0.955
_diffrn_reflns_theta_full              67.07
_diffrn_measured_fraction_theta_full   0.955
_refine_diff_density_max    0.296
_refine_diff_density_min   -0.162
_refine_diff_density_rms    0.048

