# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Delia Haynes'
'William Jones'
'W. Motherwell'
'Ze F. Weng'

_publ_contact_author_name        'Dr Delia Haynes'
_publ_contact_author_email       DHAYNES@SUN.AC.ZA

_publ_section_title              
;
The crystal structures of three novel lutidinium
pamoate salts
;

# Attachment 'B814214A.cif'

data_2_3
_database_code_depnum_ccdc_archive 'CCDC 698911'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            '2,3 lutidine pamoate'
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C7 H10 N), C23 H14 O6'
_chemical_formula_sum            'C37 H34 N2 O6'
_chemical_formula_weight         602.66

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.197(3)
_cell_length_b                   13.262(3)
_cell_length_c                   15.716(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.20(3)
_cell_angle_gamma                90.00
_cell_volume                     3025.8(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    10914
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      27.48

_exptl_crystal_description       blocks
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            19064
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.62
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6910
_reflns_number_gt                4942
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0393P)²+1.6405P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6910
_refine_ls_number_parameters     418
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_ref         0.1237
_refine_ls_wR_factor_gt          0.1073
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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
N11 N 1.22135(11) 0.11543(11) -0.01203(10) 0.0332(3) Uani 1 1 d . . .
H11N H 1.1531(18) 0.1219(19) -0.0122(16) 0.071(8) Uiso 1 1 d . . .
C12 C 1.24191(12) 0.05473(13) -0.07187(12) 0.0303(4) Uani 1 1 d . . .
C13 C 1.33325(13) 0.04705(14) -0.07281(13) 0.0355(4) Uani 1 1 d . . .
C14 C 1.39903(13) 0.10137(15) -0.00987(14) 0.0431(5) Uani 1 1 d . . .
H14 H 1.4617 0.0968 -0.0089 0.052 Uiso 1 1 calc R . .
C17 C 1.16497(13) -0.00241(15) -0.13411(13) 0.0397(4) Uani 1 1 d . . .
H17A H 1.1065 0.0175 -0.1246 0.060 Uiso 1 1 calc R . .
H17B H 1.1747 -0.0749 -0.1230 0.060 Uiso 1 1 calc R . .
H17C H 1.1631 0.0125 -0.1957 0.060 Uiso 1 1 calc R . .
C15 C 1.37585(14) 0.16196(15) 0.05143(14) 0.0434(5) Uani 1 1 d . . .
H15 H 1.4218 0.1982 0.0949 0.052 Uiso 1 1 calc R . .
C16 C 1.28533(14) 0.16869(15) 0.04814(13) 0.0397(5) Uani 1 1 d . . .
H16 H 1.2676 0.2114 0.0887 0.048 Uiso 1 1 calc R . .
C18 C 1.35715(16) -0.01855(18) -0.14087(16) 0.0543(6) Uani 1 1 d . . .
H18A H 1.4223 -0.0095 -0.1367 0.081 Uiso 1 1 calc R . .
H18B H 1.3189 0.0004 -0.2006 0.081 Uiso 1 1 calc R . .
H18C H 1.3458 -0.0893 -0.1296 0.081 Uiso 1 1 calc R . .
N21 N 0.30430(10) 0.55762(12) 0.15911(10) 0.0333(3) Uani 1 1 d . . .
H21N H 0.3515(18) 0.515(2) 0.1397(17) 0.078(8) Uiso 1 1 d . . .
C22 C 0.33526(13) 0.63052(16) 0.21968(12) 0.0391(4) Uani 1 1 d . . .
H22 H 0.3996 0.6406 0.2449 0.047 Uiso 1 1 calc R . .
C23 C 0.27450(14) 0.69010(16) 0.24512(12) 0.0418(5) Uani 1 1 d . . .
H23 H 0.2958 0.7427 0.2873 0.050 Uiso 1 1 calc R . .
C24 C 0.18135(13) 0.67255(15) 0.20842(12) 0.0378(4) Uani 1 1 d . . .
H24 H 0.1384 0.7140 0.2254 0.045 Uiso 1 1 calc R . .
C25 C 0.14954(12) 0.59605(14) 0.14770(12) 0.0318(4) Uani 1 1 d . . .
C26 C 0.21433(12) 0.53801(13) 0.12250(11) 0.0297(4) Uani 1 1 d . . .
C27 C 0.18934(14) 0.45540(15) 0.05577(14) 0.0415(5) Uani 1 1 d . . .
H27A H 0.2456 0.4239 0.0499 0.062 Uiso 1 1 calc R . .
H27B H 0.1535 0.4830 -0.0019 0.062 Uiso 1 1 calc R . .
H27C H 0.1524 0.4049 0.0753 0.062 Uiso 1 1 calc R . .
C28 C 0.04846(13) 0.57643(17) 0.10790(14) 0.0446(5) Uani 1 1 d . . .
H28A H 0.0134 0.6228 0.1340 0.067 Uiso 1 1 calc R . .
H28B H 0.0347 0.5068 0.1203 0.067 Uiso 1 1 calc R . .
H28C H 0.0313 0.5869 0.0433 0.067 Uiso 1 1 calc R . .
C311 C 0.91932(11) 0.19833(14) 0.00700(11) 0.0302(4) Uani 1 1 d . . .
C312 C 0.88177(11) 0.27039(13) 0.05425(11) 0.0277(4) Uani 1 1 d . . .
O312 O 0.94006(8) 0.33146(10) 0.11519(8) 0.0371(3) Uani 1 1 d . . .
H312 H 0.9947 0.3178 0.1177 0.056 Uiso 1 1 calc R . .
C313 C 0.78754(11) 0.28073(13) 0.03924(11) 0.0261(4) Uani 1 1 d . . .
C314 C 0.72759(11) 0.21804(13) -0.02712(11) 0.0267(4) Uani 1 1 d . . .
C315 C 0.62984(11) 0.22837(14) -0.05241(12) 0.0313(4) Uani 1 1 d . . .
H315 H 0.6027 0.2765 -0.0231 0.038 Uiso 1 1 calc R . .
C316 C 0.57457(13) 0.16944(16) -0.11870(13) 0.0391(5) Uani 1 1 d . . .
H316 H 0.5096 0.1780 -0.1349 0.047 Uiso 1 1 calc R . .
C317 C 0.61193(14) 0.09677(16) -0.16305(13) 0.0425(5) Uani 1 1 d . . .
H317 H 0.5726 0.0561 -0.2083 0.051 Uiso 1 1 calc R . .
C318 C 0.70510(13) 0.08493(15) -0.14074(13) 0.0389(4) Uani 1 1 d . . .
H318 H 0.7304 0.0357 -0.1707 0.047 Uiso 1 1 calc R . .
C319 C 0.76485(12) 0.14503(13) -0.07340(11) 0.0302(4) Uani 1 1 d . . .
C320 C 0.86136(12) 0.13713(14) -0.05443(12) 0.0322(4) Uani 1 1 d . . .
H320 H 0.8864 0.0883 -0.0850 0.039 Uiso 1 1 calc R . .
C321 C 0.75127(11) 0.36244(13) 0.08773(11) 0.0277(4) Uani 1 1 d . . .
H32A H 0.7130 0.4089 0.0424 0.033 Uiso 1 1 calc R . .
H32B H 0.8047 0.4017 0.1240 0.033 Uiso 1 1 calc R . .
C322 C 0.69477(11) 0.33005(12) 0.14850(11) 0.0250(3) Uani 1 1 d . . .
C323 C 0.60553(11) 0.36563(12) 0.13206(11) 0.0259(3) Uani 1 1 d . . .
O323 O 0.56979(8) 0.42626(10) 0.06064(8) 0.0339(3) Uani 1 1 d . . .
H323 H 0.5156 0.4423 0.0583 0.051 Uiso 1 1 calc R . .
C324 C 0.55044(11) 0.33950(12) 0.18859(11) 0.0269(4) Uani 1 1 d . . .
C325 C 0.58624(12) 0.27708(13) 0.25938(12) 0.0297(4) Uani 1 1 d . . .
H325 H 0.5489 0.2582 0.2957 0.036 Uiso 1 1 calc R . .
C326 C 0.67699(12) 0.23980(13) 0.28019(11) 0.0287(4) Uani 1 1 d . . .
C327 C 0.71411(13) 0.17649(14) 0.35479(12) 0.0353(4) Uani 1 1 d . . .
H327 H 0.6765 0.1571 0.3907 0.042 Uiso 1 1 calc R . .
C328 C 0.80273(13) 0.14291(15) 0.37603(13) 0.0389(4) Uani 1 1 d . . .
H328 H 0.8264 0.0995 0.4257 0.047 Uiso 1 1 calc R . .
C329 C 0.85884(13) 0.17309(15) 0.32374(12) 0.0360(4) Uani 1 1 d . . .
H329 H 0.9209 0.1504 0.3389 0.043 Uiso 1 1 calc R . .
C330 C 0.82569(12) 0.23464(13) 0.25127(11) 0.0302(4) Uani 1 1 d . . .
H330 H 0.8655 0.2550 0.2178 0.036 Uiso 1 1 calc R . .
C331 C 0.73270(11) 0.26854(12) 0.22528(11) 0.0261(3) Uani 1 1 d . . .
C332 C 1.02183(12) 0.19129(16) 0.02265(13) 0.0363(4) Uani 1 1 d . . .
O331 O 1.04971(9) 0.12874(13) -0.02379(11) 0.0576(4) Uani 1 1 d . . .
O332 O 1.07362(8) 0.24834(11) 0.07970(10) 0.0452(4) Uani 1 1 d . . .
C333 C 0.45549(12) 0.38308(14) 0.17424(13) 0.0328(4) Uani 1 1 d . . .
O333 O 0.40461(10) 0.34972(11) 0.21493(11) 0.0531(4) Uani 1 1 d . . .
O334 O 0.43293(9) 0.45591(11) 0.11796(10) 0.0456(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
N11 C16 1.340(2) . ?
N11 C12 1.343(2) . ?
N11 H11N 1.04(3) . ?
C12 C13 1.396(2) . ?
C12 C17 1.490(3) . ?
C13 C14 1.383(3) . ?
C13 C18 1.504(3) . ?
C14 C15 1.378(3) . ?
C14 H14 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C15 C16 1.364(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
N21 C22 1.341(2) . ?
N21 C26 1.343(2) . ?
N21 H21N 1.03(3) . ?
C22 C23 1.362(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.379(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.396(2) . ?
C25 C28 1.500(3) . ?
C26 C27 1.486(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C311 C320 1.365(3) . ?
C311 C312 1.429(2) . ?
C311 C332 1.506(2) . ?
C312 O312 1.362(2) . ?
C312 C313 1.388(2) . ?
O312 H312 0.8400 . ?
C313 C314 1.431(2) . ?
C313 C321 1.519(2) . ?
C314 C319 1.425(2) . ?
C314 C315 1.426(2) . ?
C315 C316 1.373(3) . ?
C315 H315 0.9500 . ?
C316 C317 1.404(3) . ?
C316 H316 0.9500 . ?
C317 C318 1.363(3) . ?
C317 H317 0.9500 . ?
C318 C319 1.418(3) . ?
C318 H318 0.9500 . ?
C319 C320 1.412(2) . ?
C320 H320 0.9500 . ?
C321 C322 1.523(2) . ?
C321 H32A 0.9900 . ?
C321 H32B 0.9900 . ?
C322 C323 1.386(2) . ?
C322 C331 1.429(2) . ?
C323 O323 1.357(2) . ?
C323 C324 1.432(2) . ?
O323 H323 0.8400 . ?
C324 C325 1.364(2) . ?
C324 C333 1.508(2) . ?
C325 C326 1.409(2) . ?
C325 H325 0.9500 . ?
C326 C327 1.417(2) . ?
C326 C331 1.428(2) . ?
C327 C328 1.363(3) . ?
C327 H327 0.9500 . ?
C328 C329 1.406(3) . ?
C328 H328 0.9500 . ?
C329 C330 1.370(3) . ?
C329 H329 0.9500 . ?
C330 C331 1.423(2) . ?
C330 H330 0.9500 . ?
C332 O332 1.256(2) . ?
C332 O331 1.258(2) . ?
C333 O333 1.223(2) . ?
C333 O334 1.286(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
C16 N11 C12 122.66(16) . . ?
C16 N11 H11N 118.2(14) . . ?
C12 N11 H11N 119.1(14) . . ?
N11 C12 C13 119.27(17) . . ?
N11 C12 C17 117.68(16) . . ?
C13 C12 C17 123.05(16) . . ?
C14 C13 C12 117.72(17) . . ?
C14 C13 C18 122.31(17) . . ?
C12 C13 C18 119.97(18) . . ?
C15 C14 C13 121.58(18) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C15 C14 118.37(19) . . ?
C16 C15 H15 120.8 . . ?
C14 C15 H15 120.8 . . ?
N11 C16 C15 120.37(18) . . ?
N11 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 N21 C26 122.89(16) . . ?
C22 N21 H21N 118.6(14) . . ?
C26 N21 H21N 118.6(14) . . ?
N21 C22 C23 120.05(18) . . ?
N21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C24 118.67(19) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
C25 C24 C23 121.28(18) . . ?
C25 C24 H24 119.4 . . ?
C23 C24 H24 119.4 . . ?
C24 C25 C26 118.02(17) . . ?
C24 C25 C28 121.50(17) . . ?
C26 C25 C28 120.47(17) . . ?
N21 C26 C25 119.06(17) . . ?
N21 C26 C27 117.42(16) . . ?
C25 C26 C27 123.51(16) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C320 C311 C312 119.47(15) . . ?
C320 C311 C332 119.89(16) . . ?
C312 C311 C332 120.62(16) . . ?
O312 C312 C313 118.98(15) . . ?
O312 C312 C311 119.11(15) . . ?
C313 C312 C311 121.91(16) . . ?
C312 O312 H312 109.5 . . ?
C312 C313 C314 117.98(15) . . ?
C312 C313 C321 119.65(15) . . ?
C314 C313 C321 122.21(14) . . ?
C319 C314 C315 117.47(16) . . ?
C319 C314 C313 120.23(15) . . ?
C315 C314 C313 122.24(16) . . ?
C316 C315 C314 120.66(17) . . ?
C316 C315 H315 119.7 . . ?
C314 C315 H315 119.7 . . ?
C315 C316 C317 121.41(17) . . ?
C315 C316 H316 119.3 . . ?
C317 C316 H316 119.3 . . ?
C318 C317 C316 119.55(18) . . ?
C318 C317 H317 120.2 . . ?
C316 C317 H317 120.2 . . ?
C317 C318 C319 120.94(18) . . ?
C317 C318 H318 119.5 . . ?
C319 C318 H318 119.5 . . ?
C320 C319 C318 120.78(17) . . ?
C320 C319 C314 119.17(16) . . ?
C318 C319 C314 119.96(16) . . ?
C311 C320 C319 121.20(16) . . ?
C311 C320 H320 119.4 . . ?
C319 C320 H320 119.4 . . ?
C313 C321 C322 117.96(14) . . ?
C313 C321 H32A 107.8 . . ?
C322 C321 H32A 107.8 . . ?
C313 C321 H32B 107.8 . . ?
C322 C321 H32B 107.8 . . ?
H32A C321 H32B 107.2 . . ?
C323 C322 C331 118.67(15) . . ?
C323 C322 C321 119.28(15) . . ?
C331 C322 C321 121.95(14) . . ?
O323 C323 C322 119.08(14) . . ?
O323 C323 C324 119.50(14) . . ?
C322 C323 C324 121.42(15) . . ?
C323 O323 H323 109.5 . . ?
C325 C324 C323 119.19(15) . . ?
C325 C324 C333 119.19(15) . . ?
C323 C324 C333 121.57(15) . . ?
C324 C325 C326 121.93(16) . . ?
C324 C325 H325 119.0 . . ?
C326 C325 H325 119.0 . . ?
C325 C326 C327 121.53(16) . . ?
C325 C326 C331 118.72(16) . . ?
C327 C326 C331 119.75(16) . . ?
C328 C327 C326 121.28(17) . . ?
C328 C327 H327 119.4 . . ?
C326 C327 H327 119.4 . . ?
C327 C328 C329 119.34(18) . . ?
C327 C328 H328 120.3 . . ?
C329 C328 H328 120.3 . . ?
C330 C329 C328 121.19(17) . . ?
C330 C329 H329 119.4 . . ?
C328 C329 H329 119.4 . . ?
C329 C330 C331 121.10(17) . . ?
C329 C330 H330 119.5 . . ?
C331 C330 H330 119.5 . . ?
C330 C331 C326 117.28(15) . . ?
C330 C331 C322 122.76(15) . . ?
C326 C331 C322 119.96(15) . . ?
O332 C332 O331 124.30(17) . . ?
O332 C332 C311 118.59(17) . . ?
O331 C332 C311 117.10(18) . . ?
O333 C333 O334 123.39(17) . . ?
O333 C333 C324 120.54(17) . . ?
O334 C333 C324 116.07(15) . . ?

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
C16 N11 C12 C13 -0.8(3) . . . . ?
C16 N11 C12 C17 178.67(17) . . . . ?
N11 C12 C13 C14 1.5(3) . . . . ?
C17 C12 C13 C14 -177.96(18) . . . . ?
N11 C12 C13 C18 -178.47(18) . . . . ?
C17 C12 C13 C18 2.1(3) . . . . ?
C12 C13 C14 C15 -0.6(3) . . . . ?
C18 C13 C14 C15 179.3(2) . . . . ?
C13 C14 C15 C16 -0.9(3) . . . . ?
C12 N11 C16 C15 -0.8(3) . . . . ?
C14 C15 C16 N11 1.6(3) . . . . ?
C26 N21 C22 C23 -1.5(3) . . . . ?
N21 C22 C23 C24 1.1(3) . . . . ?
C22 C23 C24 C25 0.5(3) . . . . ?
C23 C24 C25 C26 -1.5(3) . . . . ?
C23 C24 C25 C28 179.78(18) . . . . ?
C22 N21 C26 C25 0.4(3) . . . . ?
C22 N21 C26 C27 179.69(17) . . . . ?
C24 C25 C26 N21 1.1(3) . . . . ?
C28 C25 C26 N21 179.79(17) . . . . ?
C24 C25 C26 C27 -178.12(17) . . . . ?
C28 C25 C26 C27 0.6(3) . . . . ?
C320 C311 C312 O312 -179.74(15) . . . . ?
C332 C311 C312 O312 -1.3(2) . . . . ?
C320 C311 C312 C313 -0.4(3) . . . . ?
C332 C311 C312 C313 177.97(16) . . . . ?
O312 C312 C313 C314 178.01(14) . . . . ?
C311 C312 C313 C314 -1.3(2) . . . . ?
O312 C312 C313 C321 2.6(2) . . . . ?
C311 C312 C313 C321 -176.68(15) . . . . ?
C312 C313 C314 C319 2.2(2) . . . . ?
C321 C313 C314 C319 177.49(15) . . . . ?
C312 C313 C314 C315 -174.97(16) . . . . ?
C321 C313 C314 C315 0.3(2) . . . . ?
C319 C314 C315 C316 0.2(3) . . . . ?
C313 C314 C315 C316 177.53(17) . . . . ?
C314 C315 C316 C317 0.6(3) . . . . ?
C315 C316 C317 C318 -0.7(3) . . . . ?
C316 C317 C318 C319 0.0(3) . . . . ?
C317 C318 C319 C320 -175.88(18) . . . . ?
C317 C318 C319 C314 0.9(3) . . . . ?
C315 C314 C319 C320 175.85(16) . . . . ?
C313 C314 C319 C320 -1.5(2) . . . . ?
C315 C314 C319 C318 -1.0(2) . . . . ?
C313 C314 C319 C318 -178.35(16) . . . . ?
C312 C311 C320 C319 1.2(3) . . . . ?
C332 C311 C320 C319 -177.17(16) . . . . ?
C318 C319 C320 C311 176.54(17) . . . . ?
C314 C319 C320 C311 -0.3(3) . . . . ?
C312 C313 C321 C322 -119.54(17) . . . . ?
C314 C313 C321 C322 65.3(2) . . . . ?
C313 C321 C322 C323 -121.30(17) . . . . ?
C313 C321 C322 C331 62.4(2) . . . . ?
C331 C322 C323 O323 178.28(14) . . . . ?
C321 C322 C323 O323 1.9(2) . . . . ?
C331 C322 C323 C324 -1.9(2) . . . . ?
C321 C322 C323 C324 -178.36(15) . . . . ?
O323 C323 C324 C325 178.86(15) . . . . ?
C322 C323 C324 C325 -0.9(2) . . . . ?
O323 C323 C324 C333 -4.0(2) . . . . ?
C322 C323 C324 C333 176.22(15) . . . . ?
C323 C324 C325 C326 1.9(3) . . . . ?
C333 C324 C325 C326 -175.31(16) . . . . ?
C324 C325 C326 C327 178.84(17) . . . . ?
C324 C325 C326 C331 0.0(3) . . . . ?
C325 C326 C327 C328 -178.17(18) . . . . ?
C331 C326 C327 C328 0.6(3) . . . . ?
C326 C327 C328 C329 1.1(3) . . . . ?
C327 C328 C329 C330 -0.8(3) . . . . ?
C328 C329 C330 C331 -1.3(3) . . . . ?
C329 C330 C331 C326 2.9(2) . . . . ?
C329 C330 C331 C322 -177.91(17) . . . . ?
C325 C326 C331 C330 176.25(15) . . . . ?
C327 C326 C331 C330 -2.6(2) . . . . ?
C325 C326 C331 C322 -2.9(2) . . . . ?
C327 C326 C331 C322 178.22(16) . . . . ?
C323 C322 C331 C330 -175.28(16) . . . . ?
C321 C322 C331 C330 1.0(2) . . . . ?
C323 C322 C331 C326 3.8(2) . . . . ?
C321 C322 C331 C326 -179.83(15) . . . . ?
C320 C311 C332 O332 -179.85(17) . . . . ?
C312 C311 C332 O332 1.8(3) . . . . ?
C320 C311 C332 O331 1.0(3) . . . . ?
C312 C311 C332 O331 -177.35(17) . . . . ?
C325 C324 C333 O333 -13.0(3) . . . . ?
C323 C324 C333 O333 169.84(18) . . . . ?
C325 C324 C333 O334 166.76(17) . . . . ?
C323 C324 C333 O334 -10.4(2) . . . . ?

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
N11 H11N O331 1.04(3) 1.53(3) 2.566(2) 173(2) .
N21 H21N O334 1.03(3) 1.58(3) 2.609(2) 174(2) .

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.048

#=== END

data_2_4
_database_code_depnum_ccdc_archive 'CCDC 698912'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            '2,4 lutidine pamoate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H14 O6, 2(C7 H10 N)'
_chemical_formula_sum            'C37 H34 N2 O6'
_chemical_formula_weight         602.66

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'

_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                   8.2989(17)
_cell_length_b                   11.453(2)
_cell_length_c                   16.924(3)
_cell_angle_alpha                72.76(3)
_cell_angle_beta                 85.65(3)
_cell_angle_gamma                77.85(3)
_cell_volume                     1501.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    26584
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      27.48

_exptl_crystal_description       blocks
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             636
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            14633
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.53
_diffrn_reflns_theta_max         27.38
_reflns_number_total             6734
_reflns_number_gt                4009
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1489P)²+0.1269P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6734
_refine_ls_number_parameters     410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0801
_refine_ls_wR_factor_ref         0.2502
_refine_ls_wR_factor_gt          0.2129
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N11 N 0.7617(3) 0.9759(2) 0.65632(14) 0.0351(6) Uani 1 1 d . . .
H11 H 0.7530 0.9847 0.6033 0.042 Uiso 1 1 calc R . .
C12 C 0.8386(4) 1.0527(3) 0.67953(17) 0.0368(7) Uani 1 1 d . . .
C13 C 0.8539(4) 1.0363(3) 0.76295(18) 0.0403(7) Uani 1 1 d . . .
H13 H 0.9102 1.0884 0.7803 0.048 Uiso 1 1 calc R . .
C14 C 0.7880(4) 0.9446(3) 0.82219(17) 0.0390(7) Uani 1 1 d . . .
C15 C 0.7085(4) 0.8687(3) 0.79510(17) 0.0384(7) Uani 1 1 d . . .
H15 H 0.6617 0.8053 0.8336 0.046 Uiso 1 1 calc R . .
C16 C 0.6986(4) 0.8871(3) 0.71140(18) 0.0383(7) Uani 1 1 d . . .
H16 H 0.6452 0.8349 0.6925 0.046 Uiso 1 1 calc R . .
C17 C 0.8965(4) 1.1539(3) 0.61200(19) 0.0466(8) Uani 1 1 d . . .
H17A H 0.9517 1.1192 0.5683 0.070 Uiso 1 1 calc R . .
H17B H 0.9738 1.1892 0.6346 0.070 Uiso 1 1 calc R . .
H17C H 0.8017 1.2195 0.5889 0.070 Uiso 1 1 calc R . .
C18 C 0.8005(5) 0.9277(4) 0.91372(19) 0.0595(10) Uani 1 1 d . . .
H18A H 0.8881 0.9676 0.9228 0.089 Uiso 1 1 calc R . .
H18B H 0.8261 0.8385 0.9433 0.089 Uiso 1 1 calc R . .
H18C H 0.6953 0.9660 0.9344 0.089 Uiso 1 1 calc R . .
N21 N 0.6948(3) 0.4866(2) -0.15005(14) 0.0349(6) Uani 1 1 d . . .
H21 H 0.7130 0.4809 -0.0984 0.042 Uiso 1 1 calc R . .
C22 C 0.7845(4) 0.4014(2) -0.18475(16) 0.0324(6) Uani 1 1 d . . .
C23 C 0.7579(4) 0.4128(3) -0.26587(16) 0.0370(7) Uani 1 1 d . . .
H23 H 0.8216 0.3538 -0.2910 0.044 Uiso 1 1 calc R . .
C24 C 0.6402(4) 0.5085(3) -0.31214(17) 0.0381(7) Uani 1 1 d . . .
C25 C 0.5480(4) 0.5926(3) -0.27315(18) 0.0402(7) Uani 1 1 d . . .
H25 H 0.4646 0.6585 -0.3023 0.048 Uiso 1 1 calc R . .
C26 C 0.5793(4) 0.5791(3) -0.19203(17) 0.0388(7) Uani 1 1 d . . .
H26 H 0.5174 0.6367 -0.1653 0.047 Uiso 1 1 calc R . .
C27 C 0.9057(4) 0.2983(3) -0.13109(17) 0.0396(7) Uani 1 1 d . . .
H27A H 0.9469 0.3283 -0.0895 0.059 Uiso 1 1 calc R . .
H27B H 0.9979 0.2706 -0.1652 0.059 Uiso 1 1 calc R . .
H27C H 0.8516 0.2283 -0.1034 0.059 Uiso 1 1 calc R . .
C28 C 0.6147(5) 0.5224(3) -0.40211(17) 0.0513(9) Uani 1 1 d . . .
H28A H 0.6958 0.5672 -0.4363 0.077 Uiso 1 1 calc R . .
H28B H 0.5033 0.5693 -0.4181 0.077 Uiso 1 1 calc R . .
H28C H 0.6287 0.4397 -0.4104 0.077 Uiso 1 1 calc R . .
C311 C 0.6343(3) 0.6672(2) 0.13873(15) 0.0286(6) Uani 1 1 d . . .
O311 O 0.5179(2) 0.75663(17) 0.09189(11) 0.0366(5) Uani 1 1 d . . .
H311 H 0.5174 0.7459 0.0449 0.055 Uiso 1 1 calc R . .
C312 C 0.7281(3) 0.5719(2) 0.10484(15) 0.0292(6) Uani 1 1 d . . .
C313 C 0.8422(3) 0.4793(2) 0.15267(16) 0.0304(6) Uani 1 1 d . . .
H313 H 0.9063 0.4182 0.1295 0.037 Uiso 1 1 calc R . .
C314 C 0.8676(3) 0.4718(2) 0.23564(16) 0.0299(6) Uani 1 1 d . . .
C315 C 0.9792(4) 0.3713(3) 0.28580(17) 0.0363(7) Uani 1 1 d . . .
H315 H 1.0415 0.3095 0.2626 0.044 Uiso 1 1 calc R . .
C316 C 0.9994(4) 0.3614(3) 0.36711(17) 0.0407(7) Uani 1 1 d . . .
H316 H 1.0738 0.2928 0.4004 0.049 Uiso 1 1 calc R . .
C317 C 0.9085(4) 0.4541(3) 0.40102(17) 0.0393(7) Uani 1 1 d . . .
H317 H 0.9227 0.4474 0.4575 0.047 Uiso 1 1 calc R . .
C318 C 0.8001(4) 0.5535(3) 0.35422(16) 0.0345(7) Uani 1 1 d . . .
H318 H 0.7409 0.6148 0.3788 0.041 Uiso 1 1 calc R . .
C319 C 0.7745(3) 0.5669(2) 0.26942(15) 0.0284(6) Uani 1 1 d . . .
C320 C 0.6576(3) 0.6662(2) 0.21919(15) 0.0274(6) Uani 1 1 d . . .
C321 C 0.5452(3) 0.7630(2) 0.25490(16) 0.0299(6) Uani 1 1 d . . .
H32A H 0.4609 0.8116 0.2130 0.036 Uiso 1 1 calc R . .
H32B H 0.4865 0.7170 0.3034 0.036 Uiso 1 1 calc R . .
C322 C 0.6188(3) 0.8556(2) 0.28183(15) 0.0279(6) Uani 1 1 d . . .
C323 C 0.6120(3) 0.8517(2) 0.36518(15) 0.0294(6) Uani 1 1 d . . .
O323 O 0.5441(3) 0.76244(17) 0.42110(11) 0.0369(5) Uani 1 1 d . . .
H323 H 0.5476 0.7708 0.4686 0.055 Uiso 1 1 calc R . .
C324 C 0.6738(3) 0.9392(2) 0.39315(16) 0.0310(6) Uani 1 1 d . . .
C325 C 0.7274(4) 1.0366(2) 0.33617(16) 0.0332(6) Uani 1 1 d . . .
H325 H 0.7667 1.0959 0.3547 0.040 Uiso 1 1 calc R . .
C326 C 0.7257(3) 1.0506(2) 0.25074(16) 0.0315(6) Uani 1 1 d . . .
C327 C 0.7689(4) 1.1565(3) 0.19182(17) 0.0359(7) Uani 1 1 d . . .
H327 H 0.8038 1.2175 0.2106 0.043 Uiso 1 1 calc R . .
C328 C 0.7616(4) 1.1732(3) 0.10872(17) 0.0400(7) Uani 1 1 d . . .
H328 H 0.7869 1.2462 0.0699 0.048 Uiso 1 1 calc R . .
C329 C 0.7161(4) 1.0801(3) 0.08184(17) 0.0364(7) Uani 1 1 d . . .
H329 H 0.7135 1.0902 0.0241 0.044 Uiso 1 1 calc R . .
C330 C 0.6751(4) 0.9750(2) 0.13632(15) 0.0322(6) Uani 1 1 d . . .
H330 H 0.6465 0.9132 0.1160 0.039 Uiso 1 1 calc R . .
C331 C 0.6751(3) 0.9578(2) 0.22335(15) 0.0278(6) Uani 1 1 d . . .
C332 C 0.6968(4) 0.5717(3) 0.01823(16) 0.0344(7) Uani 1 1 d . . .
O331 O 0.5960(3) 0.66059(19) -0.02521(11) 0.0461(6) Uani 1 1 d . . .
O332 O 0.7742(3) 0.47990(18) -0.00530(11) 0.0422(5) Uani 1 1 d . . .
C333 C 0.6841(4) 0.9248(3) 0.48303(17) 0.0365(7) Uani 1 1 d . . .
O333 O 0.7535(3) 1.00103(19) 0.50287(11) 0.0461(6) Uani 1 1 d . . .
O334 O 0.6271(3) 0.83892(19) 0.53517(11) 0.0429(5) 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
N11 C16 1.329(4) . ?
N11 C12 1.347(4) . ?
N11 H11 0.8800 . ?
C12 C13 1.380(4) . ?
C12 C17 1.499(4) . ?
C13 C14 1.393(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(4) . ?
C14 C18 1.512(4) . ?
C15 C16 1.375(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
N21 C26 1.332(4) . ?
N21 C22 1.348(4) . ?
N21 H21 0.8800 . ?
C22 C23 1.370(4) . ?
C22 C27 1.495(4) . ?
C23 C24 1.388(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.393(4) . ?
C24 C28 1.510(4) . ?
C25 C26 1.374(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C311 O311 1.352(3) . ?
C311 C320 1.386(4) . ?
C311 C312 1.440(4) . ?
O311 H311 0.8400 . ?
C312 C313 1.364(4) . ?
C312 C332 1.509(4) . ?
C313 C314 1.411(4) . ?
C313 H313 0.9500 . ?
C314 C315 1.413(4) . ?
C314 C319 1.434(4) . ?
C315 C316 1.367(4) . ?
C315 H315 0.9500 . ?
C316 C317 1.408(4) . ?
C316 H316 0.9500 . ?
C317 C318 1.370(4) . ?
C317 H317 0.9500 . ?
C318 C319 1.425(4) . ?
C318 H318 0.9500 . ?
C319 C320 1.430(4) . ?
C320 C321 1.530(4) . ?
C321 C322 1.519(4) . ?
C321 H32A 0.9900 . ?
C321 H32B 0.9900 . ?
C322 C323 1.395(3) . ?
C322 C331 1.429(4) . ?
C323 O323 1.358(3) . ?
C323 C324 1.424(4) . ?
O323 H323 0.8400 . ?
C324 C325 1.370(4) . ?
C324 C333 1.488(4) . ?
C325 C326 1.408(4) . ?
C325 H325 0.9500 . ?
C326 C327 1.416(4) . ?
C326 C331 1.424(4) . ?
C327 C328 1.366(4) . ?
C327 H327 0.9500 . ?
C328 C329 1.403(4) . ?
C328 H328 0.9500 . ?
C329 C330 1.372(4) . ?
C329 H329 0.9500 . ?
C330 C331 1.427(3) . ?
C330 H330 0.9500 . ?
C332 O331 1.253(3) . ?
C332 O332 1.265(3) . ?
C333 O334 1.260(3) . ?
C333 O333 1.273(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
C16 N11 C12 121.8(2) . . ?
C16 N11 H11 119.1 . . ?
C12 N11 H11 119.1 . . ?
N11 C12 C13 118.5(3) . . ?
N11 C12 C17 117.0(2) . . ?
C13 C12 C17 124.4(3) . . ?
C12 C13 C14 121.1(3) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C15 C14 C13 118.2(3) . . ?
C15 C14 C18 120.3(3) . . ?
C13 C14 C18 121.6(3) . . ?
C16 C15 C14 118.7(3) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
N11 C16 C15 121.7(3) . . ?
N11 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C26 N21 C22 121.7(2) . . ?
C26 N21 H21 119.2 . . ?
C22 N21 H21 119.2 . . ?
N21 C22 C23 118.7(3) . . ?
N21 C22 C27 117.4(2) . . ?
C23 C22 C27 123.9(3) . . ?
C22 C23 C24 121.5(3) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
C23 C24 C25 117.7(3) . . ?
C23 C24 C28 121.2(3) . . ?
C25 C24 C28 121.0(3) . . ?
C26 C25 C24 119.1(3) . . ?
C26 C25 H25 120.5 . . ?
C24 C25 H25 120.5 . . ?
N21 C26 C25 121.3(3) . . ?
N21 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O311 C311 C320 119.7(2) . . ?
O311 C311 C312 119.1(2) . . ?
C320 C311 C312 121.1(2) . . ?
C311 O311 H311 109.5 . . ?
C313 C312 C311 119.4(2) . . ?
C313 C312 C332 120.1(2) . . ?
C311 C312 C332 120.4(2) . . ?
C312 C313 C314 121.8(2) . . ?
C312 C313 H313 119.1 . . ?
C314 C313 H313 119.1 . . ?
C313 C314 C315 121.1(2) . . ?
C313 C314 C319 118.8(2) . . ?
C315 C314 C319 120.1(2) . . ?
C316 C315 C314 121.2(3) . . ?
C316 C315 H315 119.4 . . ?
C314 C315 H315 119.4 . . ?
C315 C316 C317 119.3(3) . . ?
C315 C316 H316 120.4 . . ?
C317 C316 H316 120.4 . . ?
C318 C317 C316 121.3(3) . . ?
C318 C317 H317 119.4 . . ?
C316 C317 H317 119.4 . . ?
C317 C318 C319 121.3(3) . . ?
C317 C318 H318 119.4 . . ?
C319 C318 H318 119.4 . . ?
C318 C319 C320 123.2(2) . . ?
C318 C319 C314 116.9(2) . . ?
C320 C319 C314 119.8(2) . . ?
C311 C320 C319 119.0(2) . . ?
C311 C320 C321 119.2(2) . . ?
C319 C320 C321 121.5(2) . . ?
C322 C321 C320 119.7(2) . . ?
C322 C321 H32A 107.4 . . ?
C320 C321 H32A 107.4 . . ?
C322 C321 H32B 107.4 . . ?
C320 C321 H32B 107.4 . . ?
H32A C321 H32B 106.9 . . ?
C323 C322 C331 118.0(2) . . ?
C323 C322 C321 119.5(2) . . ?
C331 C322 C321 122.0(2) . . ?
O323 C323 C322 119.2(2) . . ?
O323 C323 C324 119.1(2) . . ?
C322 C323 C324 121.7(2) . . ?
C323 O323 H323 109.5 . . ?
C325 C324 C323 119.2(2) . . ?
C325 C324 C333 119.8(3) . . ?
C323 C324 C333 121.0(2) . . ?
C324 C325 C326 121.5(3) . . ?
C324 C325 H325 119.3 . . ?
C326 C325 H325 119.3 . . ?
C325 C326 C327 121.2(3) . . ?
C325 C326 C331 119.1(2) . . ?
C327 C326 C331 119.6(2) . . ?
C328 C327 C326 121.7(3) . . ?
C328 C327 H327 119.2 . . ?
C326 C327 H327 119.2 . . ?
C327 C328 C329 118.6(3) . . ?
C327 C328 H328 120.7 . . ?
C329 C328 H328 120.7 . . ?
C330 C329 C328 122.0(3) . . ?
C330 C329 H329 119.0 . . ?
C328 C329 H329 119.0 . . ?
C329 C330 C331 120.4(3) . . ?
C329 C330 H330 119.8 . . ?
C331 C330 H330 119.8 . . ?
C326 C331 C330 117.6(2) . . ?
C326 C331 C322 120.2(2) . . ?
C330 C331 C322 122.1(3) . . ?
O331 C332 O332 124.3(3) . . ?
O331 C332 C312 118.5(2) . . ?
O332 C332 C312 117.1(2) . . ?
O334 C333 O333 123.4(3) . . ?
O334 C333 C324 119.6(3) . . ?
O333 C333 C324 116.9(3) . . ?

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
C16 N11 C12 C13 1.1(4) . . . . ?
C16 N11 C12 C17 -176.6(3) . . . . ?
N11 C12 C13 C14 -1.5(4) . . . . ?
C17 C12 C13 C14 176.0(3) . . . . ?
C12 C13 C14 C15 0.9(4) . . . . ?
C12 C13 C14 C18 -178.6(3) . . . . ?
C13 C14 C15 C16 0.2(4) . . . . ?
C18 C14 C15 C16 179.6(3) . . . . ?
C12 N11 C16 C15 0.0(4) . . . . ?
C14 C15 C16 N11 -0.6(4) . . . . ?
C26 N21 C22 C23 1.5(4) . . . . ?
C26 N21 C22 C27 -177.3(3) . . . . ?
N21 C22 C23 C24 -0.8(4) . . . . ?
C27 C22 C23 C24 178.0(3) . . . . ?
C22 C23 C24 C25 -0.6(4) . . . . ?
C22 C23 C24 C28 178.4(3) . . . . ?
C23 C24 C25 C26 1.3(4) . . . . ?
C28 C24 C25 C26 -177.7(3) . . . . ?
C22 N21 C26 C25 -0.9(4) . . . . ?
C24 C25 C26 N21 -0.6(5) . . . . ?
O311 C311 C312 C313 -178.0(2) . . . . ?
C320 C311 C312 C313 -0.2(4) . . . . ?
O311 C311 C312 C332 -0.1(4) . . . . ?
C320 C311 C312 C332 177.7(2) . . . . ?
C311 C312 C313 C314 2.0(4) . . . . ?
C332 C312 C313 C314 -175.9(3) . . . . ?
C312 C313 C314 C315 176.2(3) . . . . ?
C312 C313 C314 C319 -2.2(4) . . . . ?
C313 C314 C315 C316 -177.5(3) . . . . ?
C319 C314 C315 C316 0.9(4) . . . . ?
C314 C315 C316 C317 -0.8(5) . . . . ?
C315 C316 C317 C318 0.2(5) . . . . ?
C316 C317 C318 C319 0.3(5) . . . . ?
C317 C318 C319 C320 177.2(3) . . . . ?
C317 C318 C319 C314 -0.2(4) . . . . ?
C313 C314 C319 C318 178.0(3) . . . . ?
C315 C314 C319 C318 -0.4(4) . . . . ?
C313 C314 C319 C320 0.5(4) . . . . ?
C315 C314 C319 C320 -177.9(3) . . . . ?
O311 C311 C320 C319 176.4(2) . . . . ?
C312 C311 C320 C319 -1.4(4) . . . . ?
O311 C311 C320 C321 2.9(4) . . . . ?
C312 C311 C320 C321 -174.9(2) . . . . ?
C318 C319 C320 C311 -176.1(3) . . . . ?
C314 C319 C320 C311 1.2(4) . . . . ?
C318 C319 C320 C321 -2.8(4) . . . . ?
C314 C319 C320 C321 174.5(2) . . . . ?
C311 C320 C321 C322 -118.2(3) . . . . ?
C319 C320 C321 C322 68.4(3) . . . . ?
C320 C321 C322 C323 -115.1(3) . . . . ?
C320 C321 C322 C331 73.6(3) . . . . ?
C331 C322 C323 O323 173.7(2) . . . . ?
C321 C322 C323 O323 2.0(4) . . . . ?
C331 C322 C323 C324 -6.0(4) . . . . ?
C321 C322 C323 C324 -177.7(2) . . . . ?
O323 C323 C324 C325 -173.6(2) . . . . ?
C322 C323 C324 C325 6.1(4) . . . . ?
O323 C323 C324 C333 7.7(4) . . . . ?
C322 C323 C324 C333 -172.6(2) . . . . ?
C323 C324 C325 C326 -1.2(4) . . . . ?
C333 C324 C325 C326 177.5(2) . . . . ?
C324 C325 C326 C327 175.0(3) . . . . ?
C324 C325 C326 C331 -3.3(4) . . . . ?
C325 C326 C327 C328 -177.5(3) . . . . ?
C331 C326 C327 C328 0.8(4) . . . . ?
C326 C327 C328 C329 -2.5(4) . . . . ?
C327 C328 C329 C330 1.6(5) . . . . ?
C328 C329 C330 C331 1.0(4) . . . . ?
C325 C326 C331 C330 -179.9(2) . . . . ?
C327 C326 C331 C330 1.8(4) . . . . ?
C325 C326 C331 C322 3.3(4) . . . . ?
C327 C326 C331 C322 -175.1(2) . . . . ?
C329 C330 C331 C326 -2.6(4) . . . . ?
C329 C330 C331 C322 174.1(3) . . . . ?
C323 C322 C331 C326 1.3(4) . . . . ?
C321 C322 C331 C326 172.8(2) . . . . ?
C323 C322 C331 C330 -175.3(2) . . . . ?
C321 C322 C331 C330 -3.9(4) . . . . ?
C313 C312 C332 O331 -177.3(3) . . . . ?
C311 C312 C332 O331 4.8(4) . . . . ?
C313 C312 C332 O332 3.4(4) . . . . ?
C311 C312 C332 O332 -174.5(2) . . . . ?
C325 C324 C333 O334 176.4(3) . . . . ?
C323 C324 C333 O334 -4.9(4) . . . . ?
C325 C324 C333 O333 -4.4(4) . . . . ?
C323 C324 C333 O333 174.3(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
N11 H11 O333 0.88 1.65 2.531(3) 175.2 .
N21 H21 O332 0.88 1.69 2.560(3) 170.9 .

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.38
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.098

#=== END

data_3_4
_database_code_depnum_ccdc_archive 'CCDC 698913'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            '3,4 lutidine pamoate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H14 O6, 2(C7 H10 N)'
_chemical_formula_sum            'C37 H34 N2 O6'
_chemical_formula_weight         602.66

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'

_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                   11.196(2)
_cell_length_b                   12.653(3)
_cell_length_c                   22.963(5)
_cell_angle_alpha                104.32(3)
_cell_angle_beta                 103.24(3)
_cell_angle_gamma                91.58(3)
_cell_volume                     3056.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    80454
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      25.03

_exptl_crystal_description       ?
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_T_max  1.001
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            24766
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.64
_diffrn_reflns_theta_max         25.03
_reflns_number_total             10539
_reflns_number_gt                7878
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.

The hydrogen atoms on all four lutidine ions were located in the difference
map.
;

_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)+(0.0656P)²+0.8072P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10539
_refine_ls_number_parameters     835
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1537
_refine_ls_wR_factor_gt          0.1355
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_restrained_S_all      1.162
_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
N11 N 0.65653(19) 0.05853(17) 0.51108(9) 0.0410(5) Uani 1 1 d . . .
H11 H 0.659(3) 0.005(2) 0.4704(14) 0.067(9) Uiso 1 1 d . . .
C12 C 0.7386(2) 0.0612(2) 0.56432(11) 0.0426(6) Uani 1 1 d . . .
H12 H 0.8001 0.0110 0.5640 0.051 Uiso 1 1 calc R . .
C13 C 0.7364(2) 0.1346(2) 0.61938(10) 0.0387(5) Uani 1 1 d . . .
C14 C 0.6477(2) 0.2099(2) 0.61844(10) 0.0399(6) Uani 1 1 d . . .
C15 C 0.5641(2) 0.2049(2) 0.56286(11) 0.0441(6) Uani 1 1 d . . .
H15 H 0.5028 0.2553 0.5614 0.053 Uiso 1 1 calc R . .
C16 C 0.5693(2) 0.1281(2) 0.51008(11) 0.0425(6) Uani 1 1 d . . .
H16 H 0.5103 0.1243 0.4724 0.051 Uiso 1 1 calc R . .
C17 C 0.8253(3) 0.1307(2) 0.67857(12) 0.0551(7) Uani 1 1 d . . .
H17A H 0.8625 0.2048 0.7011 0.083 Uiso 1 1 calc R . .
H17B H 0.8901 0.0837 0.6690 0.083 Uiso 1 1 calc R . .
H17C H 0.7814 0.1011 0.7042 0.083 Uiso 1 1 calc R . .
C18 C 0.6405(3) 0.2935(2) 0.67650(12) 0.0570(7) Uani 1 1 d . . .
H18A H 0.6242 0.2561 0.7069 0.086 Uiso 1 1 calc R . .
H18B H 0.5738 0.3395 0.6667 0.086 Uiso 1 1 calc R . .
H18C H 0.7188 0.3392 0.6937 0.086 Uiso 1 1 calc R . .
N21 N 0.43949(19) 0.48543(17) 0.75425(9) 0.0410(5) Uani 1 1 d . . .
H21 H 0.385(3) 0.440(2) 0.7099(14) 0.076(9) Uiso 1 1 d . . .
C22 C 0.4279(2) 0.4621(2) 0.80638(11) 0.0415(6) Uani 1 1 d . . .
H22 H 0.3728 0.4016 0.8036 0.050 Uiso 1 1 calc R . .
C23 C 0.4932(2) 0.5229(2) 0.86428(10) 0.0382(5) Uani 1 1 d . . .
C24 C 0.5706(2) 0.6131(2) 0.86724(10) 0.0395(6) Uani 1 1 d . . .
C25 C 0.5808(2) 0.6352(2) 0.81226(11) 0.0460(6) Uani 1 1 d . . .
H25 H 0.6333 0.6962 0.8133 0.055 Uiso 1 1 calc R . .
C26 C 0.5154(2) 0.5692(2) 0.75640(11) 0.0444(6) Uani 1 1 d . . .
H26 H 0.5246 0.5838 0.7190 0.053 Uiso 1 1 calc R . .
C27 C 0.4786(3) 0.4913(2) 0.92140(12) 0.0542(7) Uani 1 1 d . . .
H27A H 0.4170 0.4283 0.9095 0.081 Uiso 1 1 calc R . .
H27B H 0.4515 0.5531 0.9490 0.081 Uiso 1 1 calc R . .
H27C H 0.5577 0.4718 0.9429 0.081 Uiso 1 1 calc R . .
C28 C 0.6412(3) 0.6867(2) 0.92855(12) 0.0563(7) Uani 1 1 d . . .
H28A H 0.5839 0.7133 0.9542 0.084 Uiso 1 1 calc R . .
H28B H 0.6842 0.7490 0.9214 0.084 Uiso 1 1 calc R . .
H28C H 0.7015 0.6454 0.9498 0.084 Uiso 1 1 calc R . .
N31 N 0.05919(18) 0.12891(16) -0.00213(9) 0.0396(5) Uani 1 1 d . . .
H31 H 0.046(3) 0.180(3) 0.0409(16) 0.085(10) Uiso 1 1 d . . .
C32 C -0.0180(2) 0.1329(2) -0.05541(11) 0.0413(6) Uani 1 1 d . . .
H32 H -0.0842 0.1782 -0.0541 0.050 Uiso 1 1 calc R . .
C33 C -0.0042(2) 0.07345(19) -0.11209(10) 0.0375(5) Uani 1 1 d . . .
C34 C 0.0949(2) 0.00884(19) -0.11295(10) 0.0386(6) Uani 1 1 d . . .
C35 C 0.1724(2) 0.0061(2) -0.05699(11) 0.0437(6) Uani 1 1 d . . .
H35 H 0.2400 -0.0377 -0.0566 0.052 Uiso 1 1 calc R . .
C36 C 0.1524(2) 0.06626(19) -0.00222(10) 0.0407(6) Uani 1 1 d . . .
H36 H 0.2055 0.0631 0.0359 0.049 Uiso 1 1 calc R . .
C37 C -0.0922(2) 0.0816(2) -0.17092(11) 0.0523(7) Uani 1 1 d . . .
H37A H -0.0471 0.1121 -0.1958 0.078 Uiso 1 1 calc R . .
H37B H -0.1558 0.1295 -0.1606 0.078 Uiso 1 1 calc R . .
H37C H -0.1311 0.0086 -0.1946 0.078 Uiso 1 1 calc R . .
C38 C 0.1192(3) -0.0543(2) -0.17306(11) 0.0561(7) Uani 1 1 d . . .
H38A H 0.0487 -0.1076 -0.1961 0.084 Uiso 1 1 calc R . .
H38B H 0.1933 -0.0929 -0.1646 0.084 Uiso 1 1 calc R . .
H38C H 0.1314 -0.0037 -0.1977 0.084 Uiso 1 1 calc R . .
N41 N 0.2683(2) -0.28412(19) -0.24931(10) 0.0483(5) Uani 1 1 d . . .
H41 H 0.254(3) -0.298(3) -0.2065(16) 0.091(11) Uiso 1 1 d . . .
C42 C 0.1947(2) -0.3444(2) -0.30240(12) 0.0478(6) Uani 1 1 d . . .
H42 H 0.1288 -0.3915 -0.3007 0.057 Uiso 1 1 calc R . .
C43 C 0.2116(2) -0.3404(2) -0.35943(11) 0.0414(6) Uani 1 1 d . . .
C44 C 0.3120(2) -0.2728(2) -0.36045(11) 0.0433(6) Uani 1 1 d . . .
C45 C 0.3856(3) -0.2101(2) -0.30465(12) 0.0512(7) Uani 1 1 d . . .
H45 H 0.4530 -0.1627 -0.3046 0.061 Uiso 1 1 calc R . .
C46 C 0.3611(3) -0.2165(2) -0.24941(12) 0.0517(7) Uani 1 1 d . . .
H46 H 0.4107 -0.1724 -0.2113 0.062 Uiso 1 1 calc R . .
C47 C 0.3396(3) -0.2683(3) -0.42077(13) 0.0600(8) Uani 1 1 d . . .
H47A H 0.3523 -0.3419 -0.4435 0.090 Uiso 1 1 calc R . .
H47B H 0.4143 -0.2193 -0.4126 0.090 Uiso 1 1 calc R . .
H47C H 0.2703 -0.2407 -0.4456 0.090 Uiso 1 1 calc R . .
C48 C 0.1237(3) -0.4075(2) -0.41754(12) 0.0556(7) Uani 1 1 d . . .
H48A H 0.0770 -0.3586 -0.4395 0.083 Uiso 1 1 calc R . .
H48B H 0.0667 -0.4552 -0.4067 0.083 Uiso 1 1 calc R . .
H48C H 0.1701 -0.4523 -0.4443 0.083 Uiso 1 1 calc R . .
O111 O 0.40818(15) 0.42079(14) 0.49586(7) 0.0472(4) Uani 1 1 d . . .
H111 H 0.4363 0.4508 0.5338 0.071 Uiso 1 1 calc R . .
C111 C 0.3087(2) 0.35013(18) 0.48818(10) 0.0338(5) Uani 1 1 d . . .
C112 C 0.2697(2) 0.33629(18) 0.54066(10) 0.0332(5) Uani 1 1 d . . .
C113 C 0.1699(2) 0.26461(18) 0.53237(10) 0.0349(5) Uani 1 1 d . . .
H113 H 0.1447 0.2543 0.5675 0.042 Uiso 1 1 calc R . .
C114 C 0.1036(2) 0.20547(18) 0.47228(10) 0.0340(5) Uani 1 1 d . . .
C115 C -0.0013(2) 0.1332(2) 0.46379(11) 0.0429(6) Uani 1 1 d . . .
H115 H -0.0266 0.1231 0.4990 0.051 Uiso 1 1 calc R . .
C116 C -0.0667(2) 0.0776(2) 0.40582(12) 0.0478(6) Uani 1 1 d . . .
H116 H -0.1378 0.0302 0.4007 0.057 Uiso 1 1 calc R . .
C117 C -0.0284(2) 0.0908(2) 0.35396(11) 0.0451(6) Uani 1 1 d . . .
H117 H -0.0743 0.0522 0.3137 0.054 Uiso 1 1 calc R . .
C118 C 0.0739(2) 0.15816(19) 0.36021(10) 0.0376(5) Uani 1 1 d . . .
H118 H 0.0991 0.1640 0.3243 0.045 Uiso 1 1 calc R . .
C119 C 0.1437(2) 0.21993(17) 0.41979(10) 0.0319(5) Uani 1 1 d . . .
C120 C 0.2494(2) 0.29268(18) 0.42843(10) 0.0317(5) Uani 1 1 d . . .
C121 C 0.3036(2) 0.3053(2) 0.37509(10) 0.0362(5) Uani 1 1 d . . .
H12A H 0.3769 0.3590 0.3926 0.043 Uiso 1 1 calc R . .
H12B H 0.3329 0.2341 0.3573 0.043 Uiso 1 1 calc R . .
C122 C 0.2208(2) 0.34100(18) 0.32217(10) 0.0329(5) Uani 1 1 d . . .
O123 O 0.26513(16) 0.18341(13) 0.25367(7) 0.0458(4) Uani 1 1 d . . .
H123 H 0.2482 0.1510 0.2157 0.069 Uiso 1 1 calc R . .
C123 C 0.2051(2) 0.27530(18) 0.26239(10) 0.0346(5) Uani 1 1 d . . .
C124 C 0.1264(2) 0.30265(19) 0.21041(10) 0.0346(5) Uani 1 1 d . . .
C125 C 0.0649(2) 0.39436(19) 0.22041(10) 0.0375(5) Uani 1 1 d . . .
H125 H 0.0098 0.4108 0.1863 0.045 Uiso 1 1 calc R . .
C126 C 0.0811(2) 0.46536(19) 0.28003(10) 0.0365(5) Uani 1 1 d . . .
C127 C 0.0171(3) 0.5603(2) 0.29023(11) 0.0470(6) Uani 1 1 d . . .
H127 H -0.0388 0.5761 0.2562 0.056 Uiso 1 1 calc R . .
C128 C 0.0341(3) 0.6298(2) 0.34816(12) 0.0541(7) Uani 1 1 d . . .
H128 H -0.0110 0.6924 0.3545 0.065 Uiso 1 1 calc R . .
C129 C 0.1196(3) 0.6074(2) 0.39830(11) 0.0510(7) Uani 1 1 d . . .
H129 H 0.1341 0.6572 0.4382 0.061 Uiso 1 1 calc R . .
C130 C 0.1813(2) 0.51617(19) 0.39058(10) 0.0397(6) Uani 1 1 d . . .
H130 H 0.2382 0.5032 0.4252 0.048 Uiso 1 1 calc R . .
O131 O 0.30104(16) 0.37878(14) 0.64999(7) 0.0479(4) Uani 1 1 d . . .
C131 C 0.1624(2) 0.43943(18) 0.33148(10) 0.0339(5) Uani 1 1 d . . .
O132 O 0.42610(16) 0.46714(14) 0.61154(7) 0.0465(4) Uani 1 1 d . . .
C132 C 0.3374(2) 0.39931(19) 0.60519(10) 0.0387(6) Uani 1 1 d . . .
O133 O 0.04347(16) 0.25889(15) 0.10161(7) 0.0511(5) Uani 1 1 d . . .
C133 C 0.1138(2) 0.2312(2) 0.14596(10) 0.0386(6) Uani 1 1 d . . .
O134 O 0.17606(17) 0.14985(14) 0.13910(7) 0.0461(4) Uani 1 1 d . . .
O211 O 0.41222(15) -0.03239(14) 0.25183(7) 0.0470(4) Uani 1 1 d . . .
H211 H 0.4134 -0.0143 0.2897 0.071 Uiso 1 1 calc R . .
C211 C 0.5156(2) -0.08174(18) 0.24379(10) 0.0351(5) Uani 1 1 d . . .
C212 C 0.6042(2) -0.09675(18) 0.29625(10) 0.0345(5) Uani 1 1 d . . .
C213 C 0.7053(2) -0.15005(18) 0.28724(10) 0.0358(5) Uani 1 1 d . . .
H213 H 0.7629 -0.1621 0.3219 0.043 Uiso 1 1 calc R . .
C214 C 0.7263(2) -0.18780(18) 0.22740(10) 0.0353(5) Uani 1 1 d . . .
C215 C 0.8308(2) -0.2428(2) 0.21804(11) 0.0427(6) Uani 1 1 d . . .
H215 H 0.8881 -0.2552 0.2527 0.051 Uiso 1 1 calc R . .
C216 C 0.8517(2) -0.2787(2) 0.16044(12) 0.0492(7) Uani 1 1 d . . .
H216 H 0.9217 -0.3171 0.1549 0.059 Uiso 1 1 calc R . .
C217 C 0.7680(2) -0.2581(2) 0.10917(12) 0.0467(6) Uani 1 1 d . . .
H217 H 0.7829 -0.2818 0.0691 0.056 Uiso 1 1 calc R . .
C218 C 0.6661(2) -0.2047(2) 0.11627(10) 0.0407(6) Uani 1 1 d . . .
H218 H 0.6120 -0.1907 0.0811 0.049 Uiso 1 1 calc R . .
C219 C 0.6391(2) -0.16953(18) 0.17532(10) 0.0344(5) Uani 1 1 d . . .
C220 C 0.5312(2) -0.11792(18) 0.18428(10) 0.0348(5) Uani 1 1 d . . .
C221 C 0.4372(2) -0.09377(19) 0.13079(10) 0.0397(6) Uani 1 1 d . . .
H22A H 0.3727 -0.0546 0.1482 0.048 Uiso 1 1 calc R . .
H22B H 0.4793 -0.0422 0.1142 0.048 Uiso 1 1 calc R . .
C222 C 0.3726(2) -0.18820(19) 0.07622(10) 0.0355(5) Uani 1 1 d . . .
O223 O 0.44817(16) -0.09945(14) 0.01126(7) 0.0482(4) Uani 1 1 d . . .
H223 H 0.4429 -0.1048 -0.0265 0.072 Uiso 1 1 calc R . .
C223 C 0.3768(2) -0.1825(2) 0.01706(10) 0.0378(5) Uani 1 1 d . . .
C224 C 0.3070(2) -0.2608(2) -0.03718(10) 0.0394(6) Uani 1 1 d . . .
C225 C 0.2363(2) -0.3443(2) -0.03058(11) 0.0416(6) Uani 1 1 d . . .
H225 H 0.1883 -0.3953 -0.0666 0.050 Uiso 1 1 calc R . .
C226 C 0.2322(2) -0.3573(2) 0.02842(11) 0.0389(6) Uani 1 1 d . . .
C227 C 0.1617(2) -0.4461(2) 0.03490(12) 0.0471(6) Uani 1 1 d . . .
H227 H 0.1162 -0.4983 -0.0013 0.057 Uiso 1 1 calc R . .
C228 C 0.1571(2) -0.4592(2) 0.09153(12) 0.0510(7) Uani 1 1 d . . .
H228 H 0.1095 -0.5198 0.0949 0.061 Uiso 1 1 calc R . .
C229 C 0.2247(2) -0.3806(2) 0.14531(12) 0.0478(6) Uani 1 1 d . . .
H229 H 0.2219 -0.3887 0.1850 0.057 Uiso 1 1 calc R . .
C230 C 0.2935(2) -0.2937(2) 0.14093(11) 0.0422(6) Uani 1 1 d . . .
H230 H 0.3374 -0.2422 0.1778 0.051 Uiso 1 1 calc R . .
O231 O 0.67043(15) -0.06468(14) 0.40544(7) 0.0454(4) Uani 1 1 d . . .
C231 C 0.3016(2) -0.2778(2) 0.08250(10) 0.0368(5) Uani 1 1 d . . .
O232 O 0.49614(16) 0.00284(15) 0.36735(7) 0.0471(4) Uani 1 1 d . . .
C232 C 0.5880(2) -0.0499(2) 0.36082(10) 0.0391(6) Uani 1 1 d . . .
O233 O 0.24433(17) -0.32058(16) -0.14690(8) 0.0546(5) Uani 1 1 d . . .
C233 C 0.3118(2) -0.2507(2) -0.10075(11) 0.0441(6) Uani 1 1 d . . .
O234 O 0.38136(17) -0.17500(16) -0.10493(8) 0.0516(5) 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
N11 C16 1.333(3) . ?
N11 C12 1.343(3) . ?
N11 H11 1.02(3) . ?
C12 C13 1.377(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.396(3) . ?
C13 C17 1.502(3) . ?
C14 C15 1.385(3) . ?
C14 C18 1.503(3) . ?
C15 C16 1.367(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
N21 C26 1.324(3) . ?
N21 C22 1.334(3) . ?
N21 H21 1.07(3) . ?
C22 C23 1.383(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.392(3) . ?
C23 C27 1.504(3) . ?
C24 C25 1.387(3) . ?
C24 C28 1.508(3) . ?
C25 C26 1.373(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
N31 C36 1.327(3) . ?
N31 C32 1.340(3) . ?
N31 H31 1.08(3) . ?
C32 C33 1.378(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.397(3) . ?
C33 C37 1.507(3) . ?
C34 C35 1.385(3) . ?
C34 C38 1.502(3) . ?
C35 C36 1.370(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N41 C46 1.329(4) . ?
N41 C42 1.339(3) . ?
N41 H41 1.09(4) . ?
C42 C43 1.378(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.401(4) . ?
C43 C48 1.504(4) . ?
C44 C45 1.389(4) . ?
C44 C47 1.501(4) . ?
C45 C46 1.378(4) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
O111 C111 1.360(3) . ?
O111 H111 0.8400 . ?
C111 C120 1.384(3) . ?
C111 C112 1.419(3) . ?
C112 C113 1.366(3) . ?
C112 C132 1.508(3) . ?
C113 C114 1.416(3) . ?
C113 H113 0.9500 . ?
C114 C115 1.415(3) . ?
C114 C119 1.428(3) . ?
C115 C116 1.366(3) . ?
C115 H115 0.9500 . ?
C116 C117 1.399(4) . ?
C116 H116 0.9500 . ?
C117 C118 1.368(3) . ?
C117 H117 0.9500 . ?
C118 C119 1.428(3) . ?
C118 H118 0.9500 . ?
C119 C120 1.425(3) . ?
C120 C121 1.525(3) . ?
C121 C122 1.523(3) . ?
C121 H12A 0.9900 . ?
C121 H12B 0.9900 . ?
C122 C123 1.387(3) . ?
C122 C131 1.415(3) . ?
O123 C123 1.354(3) . ?
O123 H123 0.8400 . ?
C123 C124 1.435(3) . ?
C124 C125 1.363(3) . ?
C124 C133 1.505(3) . ?
C125 C126 1.408(3) . ?
C125 H125 0.9500 . ?
C126 C127 1.413(3) . ?
C126 C131 1.431(3) . ?
C127 C128 1.370(4) . ?
C127 H127 0.9500 . ?
C128 C129 1.412(4) . ?
C128 H128 0.9500 . ?
C129 C130 1.357(4) . ?
C129 H129 0.9500 . ?
C130 C131 1.426(3) . ?
C130 H130 0.9500 . ?
O131 C132 1.269(3) . ?
O132 C132 1.252(3) . ?
O133 C133 1.267(3) . ?
C133 O134 1.257(3) . ?
O211 C211 1.358(3) . ?
O211 H211 0.8400 . ?
C211 C220 1.382(3) . ?
C211 C212 1.431(3) . ?
C212 C213 1.364(3) . ?
C212 C232 1.509(3) . ?
C213 C214 1.415(3) . ?
C213 H213 0.9500 . ?
C214 C215 1.410(3) . ?
C214 C219 1.432(3) . ?
C215 C216 1.364(4) . ?
C215 H215 0.9500 . ?
C216 C217 1.412(4) . ?
C216 H216 0.9500 . ?
C217 C218 1.363(3) . ?
C217 H217 0.9500 . ?
C218 C219 1.423(3) . ?
C218 H218 0.9500 . ?
C219 C220 1.422(3) . ?
C220 C221 1.523(3) . ?
C221 C222 1.522(3) . ?
C221 H22A 0.9900 . ?
C221 H22B 0.9900 . ?
C222 C223 1.390(3) . ?
C222 C231 1.422(3) . ?
O223 C223 1.354(3) . ?
O223 H223 0.8400 . ?
C223 C224 1.430(3) . ?
C224 C225 1.362(4) . ?
C224 C233 1.509(3) . ?
C225 C226 1.415(3) . ?
C225 H225 0.9500 . ?
C226 C227 1.413(4) . ?
C226 C231 1.433(3) . ?
C227 C228 1.363(4) . ?
C227 H227 0.9500 . ?
C228 C229 1.418(4) . ?
C228 H228 0.9500 . ?
C229 C230 1.363(4) . ?
C229 H229 0.9500 . ?
C230 C231 1.427(3) . ?
C230 H230 0.9500 . ?
O231 C232 1.268(3) . ?
O232 C232 1.259(3) . ?
O233 C233 1.268(3) . ?
C233 O234 1.254(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
C16 N11 C12 120.4(2) . . ?
C16 N11 H11 117.9(16) . . ?
C12 N11 H11 121.8(16) . . ?
N11 C12 C13 122.1(2) . . ?
N11 C12 H12 119.0 . . ?
C13 C12 H12 119.0 . . ?
C12 C13 C14 118.0(2) . . ?
C12 C13 C17 120.4(2) . . ?
C14 C13 C17 121.6(2) . . ?
C15 C14 C13 118.6(2) . . ?
C15 C14 C18 120.3(2) . . ?
C13 C14 C18 121.1(2) . . ?
C16 C15 C14 120.5(2) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
N11 C16 C15 120.5(2) . . ?
N11 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C26 N21 C22 120.4(2) . . ?
C26 N21 H21 117.9(17) . . ?
C22 N21 H21 121.6(17) . . ?
N21 C22 C23 122.3(2) . . ?
N21 C22 H22 118.8 . . ?
C23 C22 H22 118.8 . . ?
C22 C23 C24 117.8(2) . . ?
C22 C23 C27 120.0(2) . . ?
C24 C23 C27 122.2(2) . . ?
C25 C24 C23 118.5(2) . . ?
C25 C24 C28 120.2(2) . . ?
C23 C24 C28 121.3(2) . . ?
C26 C25 C24 120.3(2) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
N21 C26 C25 120.6(2) . . ?
N21 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C36 N31 C32 120.7(2) . . ?
C36 N31 H31 120.7(17) . . ?
C32 N31 H31 118.5(17) . . ?
N31 C32 C33 122.0(2) . . ?
N31 C32 H32 119.0 . . ?
C33 C32 H32 119.0 . . ?
C32 C33 C34 118.0(2) . . ?
C32 C33 C37 120.2(2) . . ?
C34 C33 C37 121.8(2) . . ?
C35 C34 C33 118.5(2) . . ?
C35 C34 C38 120.4(2) . . ?
C33 C34 C38 121.0(2) . . ?
C36 C35 C34 120.4(2) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
N31 C36 C35 120.4(2) . . ?
N31 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C46 N41 C42 121.0(2) . . ?
C46 N41 H41 121.5(18) . . ?
C42 N41 H41 117.3(18) . . ?
N41 C42 C43 122.1(3) . . ?
N41 C42 H42 118.9 . . ?
C43 C42 H42 118.9 . . ?
C42 C43 C44 117.7(2) . . ?
C42 C43 C48 119.7(2) . . ?
C44 C43 C48 122.6(2) . . ?
C45 C44 C43 118.9(2) . . ?
C45 C44 C47 120.5(3) . . ?
C43 C44 C47 120.6(2) . . ?
C46 C45 C44 120.1(3) . . ?
C46 C45 H45 119.9 . . ?
C44 C45 H45 119.9 . . ?
N41 C46 C45 120.1(2) . . ?
N41 C46 H46 119.9 . . ?
C45 C46 H46 119.9 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C48 H48A 109.5 . . ?
C43 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C43 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C111 O111 H111 109.5 . . ?
O111 C111 C120 117.9(2) . . ?
O111 C111 C112 119.94(19) . . ?
C120 C111 C112 122.2(2) . . ?
C113 C112 C111 119.4(2) . . ?
C113 C112 C132 119.9(2) . . ?
C111 C112 C132 120.7(2) . . ?
C112 C113 C114 121.1(2) . . ?
C112 C113 H113 119.4 . . ?
C114 C113 H113 119.4 . . ?
C115 C114 C113 121.0(2) . . ?
C115 C114 C119 120.0(2) . . ?
C113 C114 C119 119.0(2) . . ?
C116 C115 C114 121.0(2) . . ?
C116 C115 H115 119.5 . . ?
C114 C115 H115 119.5 . . ?
C115 C116 C117 119.6(2) . . ?
C115 C116 H116 120.2 . . ?
C117 C116 H116 120.2 . . ?
C118 C117 C116 121.2(2) . . ?
C118 C117 H117 119.4 . . ?
C116 C117 H117 119.4 . . ?
C117 C118 C119 121.2(2) . . ?
C117 C118 H118 119.4 . . ?
C119 C118 H118 119.4 . . ?
C120 C119 C114 119.93(19) . . ?
C120 C119 C118 123.2(2) . . ?
C114 C119 C118 116.9(2) . . ?
C111 C120 C119 118.3(2) . . ?
C111 C120 C121 118.8(2) . . ?
C119 C120 C121 122.81(19) . . ?
C122 C121 C120 117.90(19) . . ?
C122 C121 H12A 107.8 . . ?
C120 C121 H12A 107.8 . . ?
C122 C121 H12B 107.8 . . ?
C120 C121 H12B 107.8 . . ?
H12A C121 H12B 107.2 . . ?
C123 C122 C131 119.1(2) . . ?
C123 C122 C121 118.2(2) . . ?
C131 C122 C121 122.69(19) . . ?
C123 O123 H123 109.5 . . ?
O123 C123 C122 118.7(2) . . ?
O123 C123 C124 120.06(19) . . ?
C122 C123 C124 121.3(2) . . ?
C125 C124 C123 119.1(2) . . ?
C125 C124 C133 121.0(2) . . ?
C123 C124 C133 120.0(2) . . ?
C124 C125 C126 121.6(2) . . ?
C124 C125 H125 119.2 . . ?
C126 C125 H125 119.2 . . ?
C125 C126 C127 121.4(2) . . ?
C125 C126 C131 119.1(2) . . ?
C127 C126 C131 119.4(2) . . ?
C128 C127 C126 121.3(2) . . ?
C128 C127 H127 119.4 . . ?
C126 C127 H127 119.4 . . ?
C127 C128 C129 119.2(2) . . ?
C127 C128 H128 120.4 . . ?
C129 C128 H128 120.4 . . ?
C130 C129 C128 121.2(2) . . ?
C130 C129 H129 119.4 . . ?
C128 C129 H129 119.4 . . ?
C129 C130 C131 121.2(2) . . ?
C129 C130 H130 119.4 . . ?
C131 C130 H130 119.4 . . ?
C122 C131 C130 122.9(2) . . ?
C122 C131 C126 119.68(19) . . ?
C130 C131 C126 117.5(2) . . ?
O132 C132 O131 124.1(2) . . ?
O132 C132 C112 118.7(2) . . ?
O131 C132 C112 117.2(2) . . ?
O134 C133 O133 124.0(2) . . ?
O134 C133 C124 118.4(2) . . ?
O133 C133 C124 117.6(2) . . ?
C211 O211 H211 109.5 . . ?
O211 C211 C220 118.5(2) . . ?
O211 C211 C212 119.8(2) . . ?
C220 C211 C212 121.7(2) . . ?
C213 C212 C211 119.2(2) . . ?
C213 C212 C232 120.6(2) . . ?
C211 C212 C232 120.1(2) . . ?
C212 C213 C214 121.4(2) . . ?
C212 C213 H213 119.3 . . ?
C214 C213 H213 119.3 . . ?
C215 C214 C213 121.5(2) . . ?
C215 C214 C219 119.5(2) . . ?
C213 C214 C219 119.0(2) . . ?
C216 C215 C214 121.6(2) . . ?
C216 C215 H215 119.2 . . ?
C214 C215 H215 119.2 . . ?
C215 C216 C217 119.2(2) . . ?
C215 C216 H216 120.4 . . ?
C217 C216 H216 120.4 . . ?
C218 C217 C216 121.1(2) . . ?
C218 C217 H217 119.5 . . ?
C216 C217 H217 119.5 . . ?
C217 C218 C219 121.3(2) . . ?
C217 C218 H218 119.4 . . ?
C219 C218 H218 119.4 . . ?
C220 C219 C218 123.0(2) . . ?
C220 C219 C214 119.6(2) . . ?
C218 C219 C214 117.3(2) . . ?
C211 C220 C219 119.0(2) . . ?
C211 C220 C221 119.1(2) . . ?
C219 C220 C221 121.8(2) . . ?
C222 C221 C220 119.25(19) . . ?
C222 C221 H22A 107.5 . . ?
C220 C221 H22A 107.5 . . ?
C222 C221 H22B 107.5 . . ?
C220 C221 H22B 107.5 . . ?
H22A C221 H22B 107.0 . . ?
C223 C222 C231 118.6(2) . . ?
C223 C222 C221 118.0(2) . . ?
C231 C222 C221 123.3(2) . . ?
C223 O223 H223 109.5 . . ?
O223 C223 C222 118.5(2) . . ?
O223 C223 C224 119.7(2) . . ?
C222 C223 C224 121.8(2) . . ?
C225 C224 C223 119.1(2) . . ?
C225 C224 C233 120.6(2) . . ?
C223 C224 C233 120.3(2) . . ?
C224 C225 C226 121.9(2) . . ?
C224 C225 H225 119.1 . . ?
C226 C225 H225 119.1 . . ?
C227 C226 C225 121.6(2) . . ?
C227 C226 C231 119.8(2) . . ?
C225 C226 C231 118.6(2) . . ?
C228 C227 C226 122.0(2) . . ?
C228 C227 H227 119.0 . . ?
C226 C227 H227 119.0 . . ?
C227 C228 C229 118.6(3) . . ?
C227 C228 H228 120.7 . . ?
C229 C228 H228 120.7 . . ?
C230 C229 C228 121.1(2) . . ?
C230 C229 H229 119.5 . . ?
C228 C229 H229 119.5 . . ?
C229 C230 C231 121.9(2) . . ?
C229 C230 H230 119.1 . . ?
C231 C230 H230 119.1 . . ?
C222 C231 C230 123.4(2) . . ?
C222 C231 C226 120.0(2) . . ?
C230 C231 C226 116.6(2) . . ?
O232 C232 O231 124.1(2) . . ?
O232 C232 C212 118.7(2) . . ?
O231 C232 C212 117.1(2) . . ?
O234 C233 O233 124.1(2) . . ?
O234 C233 C224 118.7(2) . . ?
O233 C233 C224 117.1(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
N11 H11 O231 1.02(3) 1.57(3) 2.580(3) 173(3) .
N21 H21 O131 1.07(3) 1.49(3) 2.558(3) 176(3) .
N31 H31 O133 1.08(3) 1.51(3) 2.585(3) 173(3) .
N41 H41 O233 1.09(4) 1.49(4) 2.576(3) 176(3) .
O111 H111 O111 0.84 2.66 2.773(3) 88.9 2_666

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.106



