# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Dr Yoshitane Imai'
_publ_contact_author_email       y-imai@apch.kindai.ac.jp

_publ_section_title              
;
Polymorphic supramolecular organic
fluorophore composed of 2-naphthalenecarboxylic acid
and benzylamine
;
loop_
_publ_author_name
Yu.Kobayashi
T.Kinuta
T.Sato
T.Harada
R.Kuroda
Y.Matsubara
;
Y.Imai
;

# Attachment '- IMAI813Ver3.CIF'

data_imai813V2_1
_database_code_depnum_ccdc_archive 'CCDC 815983'
#TrackingRef '- IMAI813Ver3.CIF'

#data_im8695a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H17 N O2'
_chemical_formula_weight         279.33

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   6.2850(3)
_cell_length_b                   8.3874(4)
_cell_length_c                   27.2578(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1436.89(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    1863
_cell_measurement_theta_min      1.49
_cell_measurement_theta_max      27.88

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             592
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9631
_exptl_absorpt_correction_T_max  0.9834
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12758
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         27.88
_reflns_number_total             1952
_reflns_number_gt                1863
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0544P)^2^+0.2109P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_number_reflns         1952
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0896
_refine_ls_wR_factor_gt          0.0883
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

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
C1 C 0.8962(2) -0.02622(19) 0.16737(5) 0.0186(3) Uani 1 1 d . . .
H1 H 1.0342 0.0177 0.1719 0.022 Uiso 1 1 calc R . .
C2 C 0.7990(2) -0.01322(18) 0.12253(5) 0.0172(3) Uani 1 1 d . . .
C3 C 0.5931(2) -0.07757(18) 0.11571(5) 0.0191(3) Uani 1 1 d . . .
H3 H 0.5245 -0.0666 0.0848 0.023 Uiso 1 1 calc R . .
C4 C 0.4919(3) -0.15540(19) 0.15313(5) 0.0210(3) Uani 1 1 d . . .
H4 H 0.3542 -0.1988 0.1479 0.025 Uiso 1 1 calc R . .
C5 C 0.4916(3) -0.2546(2) 0.23896(5) 0.0258(4) Uani 1 1 d . . .
H5 H 0.3558 -0.3020 0.2343 0.031 Uiso 1 1 calc R . .
C6 C 0.5904(3) -0.2663(2) 0.28353(6) 0.0288(4) Uani 1 1 d . . .
H6 H 0.5233 -0.3226 0.3095 0.035 Uiso 1 1 calc R . .
C7 C 0.7917(3) -0.1953(2) 0.29120(6) 0.0267(4) Uani 1 1 d . . .
H7 H 0.8575 -0.2025 0.3225 0.032 Uiso 1 1 calc R . .
C8 C 0.8922(3) -0.11647(19) 0.25406(5) 0.0229(3) Uani 1 1 d . . .
H8 H 1.0278 -0.0698 0.2596 0.027 Uiso 1 1 calc R . .
C9 C 0.7945(2) -0.10389(18) 0.20705(5) 0.0183(3) Uani 1 1 d . . .
C10 C 0.5901(3) -0.17210(19) 0.19967(5) 0.0194(3) Uani 1 1 d . . .
C11 C 0.9154(2) 0.06451(18) 0.08028(5) 0.0186(3) Uani 1 1 d . . .
O12 O 1.10781(18) 0.09470(16) 0.08577(4) 0.0286(3) Uani 1 1 d . . .
O13 O 0.80954(17) 0.09161(14) 0.04164(4) 0.0219(2) Uani 1 1 d . . .
C21 C 1.1603(2) 0.0305(2) -0.07852(5) 0.0213(3) Uani 1 1 d . . .
C22 C 1.2175(3) -0.0421(2) -0.03465(6) 0.0243(3) Uani 1 1 d . . .
H22 H 1.1320 -0.0273 -0.0063 0.029 Uiso 1 1 calc R . .
C23 C 1.3985(3) -0.1359(2) -0.03204(6) 0.0281(4) Uani 1 1 d . . .
H23 H 1.4380 -0.1833 -0.0017 0.034 Uiso 1 1 calc R . .
C24 C 1.5225(3) -0.1611(2) -0.07342(6) 0.0270(4) Uani 1 1 d . . .
H24 H 1.6454 -0.2268 -0.0716 0.032 Uiso 1 1 calc R . .
C25 C 1.4658(3) -0.0900(2) -0.11727(6) 0.0267(4) Uani 1 1 d . . .
H25 H 1.5499 -0.1068 -0.1458 0.032 Uiso 1 1 calc R . .
C26 C 1.2861(3) 0.0061(2) -0.11974(6) 0.0248(3) Uani 1 1 d . . .
H26 H 1.2489 0.0556 -0.1499 0.030 Uiso 1 1 calc R . .
C27 C 0.9601(3) 0.1279(2) -0.08313(6) 0.0261(4) Uani 1 1 d . . .
H27A H 0.9632 0.1857 -0.1148 0.031 Uiso 1 1 calc R . .
H27B H 0.8364 0.0549 -0.0838 0.031 Uiso 1 1 calc R . .
N28 N 0.9301(2) 0.24488(16) -0.04297(4) 0.0198(3) Uani 1 1 d . . .
H28A H 0.9082 0.1921 -0.0142 0.030 Uiso 1 1 calc R . .
H28B H 0.8154 0.3074 -0.0497 0.030 Uiso 1 1 calc R . .
H28C H 1.0483 0.3070 -0.0403 0.030 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0161(6) 0.0189(7) 0.0209(7) -0.0003(6) 0.0018(5) -0.0010(6)
C2 0.0188(7) 0.0163(6) 0.0165(6) 0.0007(6) 0.0038(6) 0.0009(6)
C3 0.0192(7) 0.0207(7) 0.0174(6) 0.0006(6) -0.0016(6) -0.0003(6)
C4 0.0192(7) 0.0228(8) 0.0211(7) -0.0012(6) 0.0007(6) -0.0052(6)
C5 0.0317(8) 0.0239(8) 0.0219(7) 0.0005(6) 0.0060(7) -0.0072(8)
C6 0.0443(10) 0.0229(8) 0.0191(7) 0.0028(6) 0.0089(7) -0.0028(8)
C7 0.0399(10) 0.0234(8) 0.0168(7) 0.0008(6) -0.0019(7) 0.0044(8)
C8 0.0258(8) 0.0231(7) 0.0197(7) -0.0011(6) -0.0020(6) 0.0021(7)
C9 0.0208(7) 0.0171(7) 0.0170(6) -0.0001(6) 0.0000(6) 0.0026(6)
C10 0.0218(7) 0.0180(7) 0.0183(6) -0.0008(6) 0.0036(6) -0.0004(7)
C11 0.0195(7) 0.0179(7) 0.0185(6) 0.0022(6) 0.0042(6) 0.0010(6)
O12 0.0196(5) 0.0408(7) 0.0256(5) 0.0082(5) 0.0023(5) -0.0065(6)
O13 0.0207(5) 0.0276(6) 0.0172(5) 0.0066(4) 0.0028(4) 0.0037(5)
C21 0.0219(7) 0.0208(7) 0.0212(7) -0.0030(6) -0.0022(6) -0.0039(6)
C22 0.0279(8) 0.0247(8) 0.0204(7) -0.0028(6) 0.0021(6) 0.0009(7)
C23 0.0378(9) 0.0241(8) 0.0224(7) 0.0004(7) -0.0021(7) 0.0046(7)
C24 0.0262(8) 0.0204(8) 0.0344(8) -0.0038(7) 0.0005(7) 0.0029(7)
C25 0.0288(8) 0.0256(8) 0.0256(7) -0.0027(7) 0.0075(7) -0.0029(7)
C26 0.0288(8) 0.0259(8) 0.0198(7) 0.0008(6) 0.0010(7) -0.0042(7)
C27 0.0214(7) 0.0343(9) 0.0225(7) -0.0032(7) -0.0062(6) 0.0008(7)
N28 0.0152(6) 0.0252(6) 0.0191(6) 0.0056(5) 0.0005(5) 0.0009(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.3706(19) . ?
C1 C9 1.415(2) . ?
C2 C3 1.414(2) . ?
C2 C11 1.5118(19) . ?
C3 C4 1.368(2) . ?
C4 C10 1.418(2) . ?
C5 C6 1.368(2) . ?
C5 C10 1.417(2) . ?
C6 C7 1.414(3) . ?
C7 C8 1.364(2) . ?
C8 C9 1.4247(19) . ?
C9 C10 1.421(2) . ?
C11 O12 1.245(2) . ?
C11 O13 1.2663(18) . ?
C21 C22 1.389(2) . ?
C21 C26 1.389(2) . ?
C21 C27 1.506(2) . ?
C22 C23 1.385(2) . ?
C23 C24 1.387(2) . ?
C24 C25 1.383(2) . ?
C25 C26 1.389(2) . ?
C27 N28 1.482(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 C1 C9 121.14(14) . . ?
C1 C2 C3 119.63(13) . . ?
C1 C2 C11 119.87(13) . . ?
C3 C2 C11 120.46(13) . . ?
C4 C3 C2 120.65(14) . . ?
C3 C4 C10 120.78(14) . . ?
C6 C5 C10 120.51(16) . . ?
C5 C6 C7 120.49(15) . . ?
C8 C7 C6 120.56(15) . . ?
C7 C8 C9 120.27(16) . . ?
C1 C9 C10 119.05(13) . . ?
C1 C9 C8 121.82(14) . . ?
C10 C9 C8 119.14(14) . . ?
C5 C10 C4 122.28(14) . . ?
C5 C10 C9 119.00(14) . . ?
C4 C10 C9 118.72(13) . . ?
O12 C11 O13 125.02(14) . . ?
O12 C11 C2 117.78(14) . . ?
O13 C11 C2 117.19(13) . . ?
C22 C21 C26 118.98(15) . . ?
C22 C21 C27 121.74(14) . . ?
C26 C21 C27 119.21(14) . . ?
C23 C22 C21 120.38(15) . . ?
C22 C23 C24 120.42(15) . . ?
C25 C24 C23 119.49(16) . . ?
C24 C25 C26 120.12(15) . . ?
C21 C26 C25 120.59(15) . . ?
N28 C27 C21 113.83(13) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        27.88
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.040

#===END

data_imai813V2_2
_database_code_depnum_ccdc_archive 'CCDC 815984'
#TrackingRef '- IMAI813Ver3.CIF'

#data_im0570a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H17 N O2'
_chemical_formula_weight         279.33
_chemical_absolute_configration  rm

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           orthorhombic
_symmetry_space_group_name_H-M   P21

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

_cell_length_a                   9.607(2)
_cell_length_b                   5.9725(14)
_cell_length_c                   13.838(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.434(3)
_cell_angle_gamma                90.00
_cell_volume                     744.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3457
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      31.00

_exptl_crystal_description       platelet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             296
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9605
_exptl_absorpt_correction_T_max  0.9919
_exptl_absorpt_process_details   multi-scan

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6098
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         31.00
_reflns_number_total             3609
_reflns_number_gt                3457
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0700P)^2^+0.1830P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(12)
_refine_ls_number_reflns         3609
_refine_ls_number_parameters     191
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1198
_refine_ls_wR_factor_gt          0.1182
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
C1 C 1.00094(16) 0.4467(3) 0.30549(11) 0.0194(3) Uani 1 1 d . . .
H1 H 1.0149 0.3034 0.2805 0.023 Uiso 1 1 calc R . .
C2 C 0.86920(16) 0.5587(3) 0.25921(11) 0.0183(3) Uani 1 1 d . . .
C3 C 0.84850(16) 0.7725(3) 0.29611(12) 0.0200(3) Uani 1 1 d . . .
H3 H 0.7582 0.8510 0.2635 0.024 Uiso 1 1 calc R . .
C4 C 0.95735(18) 0.8679(3) 0.37846(12) 0.0217(3) Uani 1 1 d . . .
H4 H 0.9409 1.0108 0.4027 0.026 Uiso 1 1 calc R . .
C5 C 1.20866(19) 0.8500(3) 0.51323(12) 0.0246(3) Uani 1 1 d . . .
H5 H 1.1944 0.9914 0.5398 0.030 Uiso 1 1 calc R . .
C6 C 1.34098(19) 0.7367(3) 0.55778(13) 0.0300(4) Uani 1 1 d . . .
H6 H 1.4172 0.8003 0.6150 0.036 Uiso 1 1 calc R . .
C7 C 1.36367(19) 0.5264(3) 0.51876(13) 0.0301(4) Uani 1 1 d . . .
H7 H 1.4556 0.4507 0.5496 0.036 Uiso 1 1 calc R . .
C8 C 1.25446(17) 0.4302(3) 0.43685(12) 0.0238(3) Uani 1 1 d . . .
H8 H 1.2710 0.2887 0.4114 0.029 Uiso 1 1 calc R . .
C9 C 1.11655(16) 0.5422(3) 0.39006(11) 0.0193(3) Uani 1 1 d . . .
C10 C 1.09377(17) 0.7560(3) 0.42777(11) 0.0196(3) Uani 1 1 d . . .
C11 C 0.74776(17) 0.4497(3) 0.17091(12) 0.0216(3) Uani 1 1 d . . .
O12 O 0.76814(14) 0.2529(2) 0.14810(10) 0.0326(3) Uani 1 1 d . . .
O13 O 0.63139(12) 0.5655(2) 0.12630(9) 0.0259(3) Uani 1 1 d . . .
C21 C 0.26363(18) 0.2076(3) 0.10725(13) 0.0233(3) Uani 1 1 d . . .
C22 C 0.39971(18) 0.1007(3) 0.15211(13) 0.0271(3) Uani 1 1 d . . .
H22 H 0.4844 0.1533 0.1385 0.032 Uiso 1 1 calc R . .
C23 C 0.4128(2) -0.0829(3) 0.21682(14) 0.0307(4) Uani 1 1 d . . .
H23 H 0.5058 -0.1566 0.2460 0.037 Uiso 1 1 calc R . .
C24 C 0.2904(2) -0.1586(3) 0.23886(14) 0.0311(4) Uani 1 1 d . . .
H24 H 0.2998 -0.2824 0.2838 0.037 Uiso 1 1 calc R . .
C25 C 0.15486(19) -0.0526(3) 0.19494(13) 0.0297(4) Uani 1 1 d . . .
H25 H 0.0708 -0.1044 0.2095 0.036 Uiso 1 1 calc R . .
C26 C 0.14093(18) 0.1290(3) 0.12974(13) 0.0263(3) Uani 1 1 d . . .
H26 H 0.0474 0.2007 0.1001 0.032 Uiso 1 1 calc R . .
C27 C 0.24130(19) 0.4089(3) 0.03793(14) 0.0286(4) Uani 1 1 d . . .
H27A H 0.1435 0.3959 -0.0180 0.034 Uiso 1 1 calc R . .
H27B H 0.2389 0.5447 0.0783 0.034 Uiso 1 1 calc R . .
N27 N 0.35750(15) 0.4378(2) -0.00886(10) 0.0232(3) Uani 1 1 d . . .
H27C H 0.3626 0.3121 -0.0446 0.035 Uiso 1 1 calc R . .
H27D H 0.4468 0.4619 0.0418 0.035 Uiso 1 1 calc R . .
H27E H 0.3343 0.5572 -0.0524 0.035 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0195(7) 0.0184(7) 0.0204(6) 0.0005(6) 0.0072(5) -0.0008(6)
C2 0.0191(6) 0.0186(6) 0.0176(6) 0.0001(5) 0.0067(5) -0.0017(5)
C3 0.0180(6) 0.0196(7) 0.0231(7) 0.0012(6) 0.0083(5) 0.0018(6)
C4 0.0247(8) 0.0202(7) 0.0228(7) -0.0012(6) 0.0116(6) 0.0008(6)
C5 0.0254(8) 0.0255(7) 0.0223(7) -0.0037(6) 0.0076(6) -0.0075(6)
C6 0.0255(8) 0.0381(10) 0.0226(7) 0.0008(7) 0.0037(6) -0.0079(7)
C7 0.0207(7) 0.0397(10) 0.0265(7) 0.0062(7) 0.0041(6) 0.0017(7)
C8 0.0221(7) 0.0251(7) 0.0239(7) 0.0034(7) 0.0077(6) 0.0020(6)
C9 0.0183(6) 0.0214(7) 0.0187(6) 0.0024(6) 0.0070(5) 0.0006(6)
C10 0.0212(7) 0.0194(7) 0.0191(6) 0.0010(6) 0.0083(5) -0.0019(6)
C11 0.0203(7) 0.0217(7) 0.0209(6) 0.0002(6) 0.0049(5) -0.0055(6)
O12 0.0322(6) 0.0246(6) 0.0328(6) -0.0065(5) 0.0012(5) -0.0009(5)
O13 0.0202(5) 0.0278(6) 0.0257(5) 0.0025(5) 0.0031(4) -0.0015(5)
C21 0.0204(7) 0.0241(8) 0.0254(7) -0.0018(6) 0.0080(6) -0.0015(6)
C22 0.0189(7) 0.0332(9) 0.0309(8) 0.0052(7) 0.0107(6) 0.0008(6)
C23 0.0235(8) 0.0361(9) 0.0323(8) 0.0076(8) 0.0095(6) 0.0031(7)
C24 0.0324(9) 0.0351(9) 0.0288(8) 0.0061(8) 0.0144(7) -0.0011(8)
C25 0.0246(8) 0.0370(10) 0.0313(8) -0.0001(8) 0.0146(6) -0.0032(7)
C26 0.0192(7) 0.0325(9) 0.0278(8) -0.0030(7) 0.0088(6) -0.0007(6)
C27 0.0226(7) 0.0284(9) 0.0361(8) 0.0030(7) 0.0118(6) 0.0034(6)
N27 0.0214(6) 0.0206(6) 0.0251(6) 0.0013(5) 0.0049(5) -0.0001(5)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.376(2) . ?
C1 C9 1.422(2) . ?
C2 C3 1.415(2) . ?
C2 C11 1.511(2) . ?
C3 C4 1.373(2) . ?
C4 C10 1.416(2) . ?
C5 C6 1.381(2) . ?
C5 C10 1.422(2) . ?
C6 C7 1.414(3) . ?
C7 C8 1.373(2) . ?
C8 C9 1.422(2) . ?
C9 C10 1.425(2) . ?
C11 O12 1.250(2) . ?
C11 O13 1.276(2) . ?
C21 C22 1.391(2) . ?
C21 C26 1.401(2) . ?
C21 C27 1.506(2) . ?
C22 C23 1.393(3) . ?
C23 C24 1.389(2) . ?
C24 C25 1.384(3) . ?
C25 C26 1.387(3) . ?
C27 N27 1.483(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 C1 C9 121.03(14) . . ?
C1 C2 C3 119.53(13) . . ?
C1 C2 C11 119.48(13) . . ?
C3 C2 C11 120.98(13) . . ?
C4 C3 C2 120.79(14) . . ?
C3 C4 C10 120.84(14) . . ?
C6 C5 C10 120.25(16) . . ?
C5 C6 C7 120.39(15) . . ?
C8 C7 C6 120.76(16) . . ?
C7 C8 C9 120.07(16) . . ?
C1 C9 C8 121.46(14) . . ?
C1 C9 C10 119.03(13) . . ?
C8 C9 C10 119.50(14) . . ?
C4 C10 C5 122.24(15) . . ?
C4 C10 C9 118.76(13) . . ?
C5 C10 C9 119.00(14) . . ?
O12 C11 O13 125.15(14) . . ?
O12 C11 C2 117.69(14) . . ?
O13 C11 C2 117.16(14) . . ?
C22 C21 C26 118.66(15) . . ?
C22 C21 C27 123.60(14) . . ?
C26 C21 C27 117.72(15) . . ?
C21 C22 C23 120.54(15) . . ?
C24 C23 C22 120.23(17) . . ?
C25 C24 C23 119.59(17) . . ?
C24 C25 C26 120.39(16) . . ?
C25 C26 C21 120.59(16) . . ?
N27 C27 C21 114.16(13) . . ?

_diffrn_measured_fraction_theta_max 0.829
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.950
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.048

#===END

data_imai813V2_3
_database_code_depnum_ccdc_archive 'CCDC 815985'
#TrackingRef '- IMAI813Ver3.CIF'

#data_im0577a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H25 N O4'
_chemical_formula_weight         451.50

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   P21/c

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

_cell_length_a                   12.633(2)
_cell_length_b                   6.0545(11)
_cell_length_c                   31.019(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.008(3)
_cell_angle_gamma                90.00
_cell_volume                     2320.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5933
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      31.01

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9542
_exptl_absorpt_correction_T_max  0.9872
_exptl_absorpt_process_details   multi-scan

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19734
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         2.69
_diffrn_reflns_theta_max         31.01
_reflns_number_total             6636
_reflns_number_gt                5933
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0620P)^2^+0.6874P] where P=(Fo^2^+2Fc^2^)/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         6636
_refine_ls_number_parameters     309
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1147
_refine_ls_wR_factor_gt          0.1104
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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
C1 C 0.33317(7) -0.18976(15) 0.11801(3) 0.01643(17) Uani 1 1 d . . .
H1 H 0.3101 -0.3257 0.1283 0.020 Uiso 1 1 calc R . .
C2 C 0.28744(7) -0.11741(15) 0.07623(3) 0.01432(16) Uani 1 1 d . . .
C3 C 0.32329(7) 0.08427(15) 0.06058(3) 0.01633(17) Uani 1 1 d . . .
H3 H 0.2933 0.1325 0.0315 0.020 Uiso 1 1 calc R . .
C4 C 0.40083(7) 0.20978(16) 0.08721(3) 0.01789(17) Uani 1 1 d . . .
H4 H 0.4232 0.3452 0.0764 0.021 Uiso 1 1 calc R . .
C5 C 0.52905(8) 0.26540(17) 0.15900(3) 0.0222(2) Uani 1 1 d . . .
H5 H 0.5521 0.4024 0.1492 0.027 Uiso 1 1 calc R . .
C6 C 0.57418(8) 0.1903(2) 0.20045(4) 0.0254(2) Uani 1 1 d . . .
H6 H 0.6283 0.2754 0.2191 0.030 Uiso 1 1 calc R . .
C7 C 0.54067(8) -0.01317(19) 0.21574(3) 0.0254(2) Uani 1 1 d . . .
H7 H 0.5724 -0.0639 0.2445 0.030 Uiso 1 1 calc R . .
C8 C 0.46243(8) -0.13727(18) 0.18910(3) 0.02210(19) Uani 1 1 d . . .
H8 H 0.4402 -0.2734 0.1996 0.027 Uiso 1 1 calc R . .
C9 C 0.41447(7) -0.06403(16) 0.14603(3) 0.01710(17) Uani 1 1 d . . .
C10 C 0.44804(7) 0.14012(16) 0.13056(3) 0.01725(17) Uani 1 1 d . . .
C11 C 0.19731(7) -0.24505(14) 0.04768(3) 0.01319(16) Uani 1 1 d . . .
O12 O 0.17355(5) -0.43517(11) 0.05984(2) 0.01769(14) Uani 1 1 d . . .
O13 O 0.14794(5) -0.15851(11) 0.01200(2) 0.01474(13) Uani 1 1 d . . .
C21 C 0.17308(7) 0.15218(15) 0.21106(3) 0.01591(17) Uani 1 1 d . . .
H21 H 0.2078 0.2915 0.2114 0.019 Uiso 1 1 calc R . .
C22 C 0.12487(7) 0.05822(15) 0.17142(3) 0.01580(17) Uani 1 1 d . . .
C23 C 0.07549(8) -0.15270(16) 0.17048(3) 0.01828(18) Uani 1 1 d . . .
H23 H 0.0430 -0.2176 0.1430 0.022 Uiso 1 1 calc R . .
C24 C 0.07434(8) -0.26333(15) 0.20894(3) 0.01854(18) Uani 1 1 d . . .
H24 H 0.0420 -0.4054 0.2079 0.022 Uiso 1 1 calc R . .
C25 C 0.11729(8) -0.27394(16) 0.29092(3) 0.02032(19) Uani 1 1 d . . .
H25 H 0.0840 -0.4148 0.2907 0.024 Uiso 1 1 calc R . .
C26 C 0.16130(8) -0.17487(18) 0.33030(3) 0.0229(2) Uani 1 1 d . . .
H26 H 0.1576 -0.2471 0.3571 0.028 Uiso 1 1 calc R . .
C27 C 0.21209(8) 0.03369(18) 0.33139(3) 0.02192(19) Uani 1 1 d . . .
H27 H 0.2428 0.1000 0.3589 0.026 Uiso 1 1 calc R . .
C28 C 0.21734(8) 0.14099(16) 0.29283(3) 0.01903(18) Uani 1 1 d . . .
H28 H 0.2517 0.2810 0.2938 0.023 Uiso 1 1 calc R . .
C29 C 0.17149(7) 0.04349(15) 0.25143(3) 0.01588(17) Uani 1 1 d . . .
C30 C 0.12107(7) -0.16750(15) 0.25040(3) 0.01638(17) Uani 1 1 d . . .
C31 C 0.12019(7) 0.17876(15) 0.12910(3) 0.01653(17) Uani 1 1 d . . .
O32 O 0.18331(6) 0.35542(12) 0.13369(2) 0.02246(16) Uani 1 1 d . . .
H32 H 0.1778 0.4182 0.1092 0.034 Uiso 1 1 calc R . .
O33 O 0.06311(6) 0.12184(13) 0.09404(2) 0.02219(15) Uani 1 1 d . . .
C41 C 0.19848(7) 0.30248(15) -0.05401(3) 0.01536(17) Uani 1 1 d . . .
C42 C 0.27316(7) 0.47305(16) -0.04289(3) 0.01804(18) Uani 1 1 d . . .
H42 H 0.2510 0.6103 -0.0328 0.022 Uiso 1 1 calc R . .
C43 C 0.38032(8) 0.44250(18) -0.04647(3) 0.0231(2) Uani 1 1 d . . .
H43 H 0.4312 0.5586 -0.0386 0.028 Uiso 1 1 calc R . .
C44 C 0.41301(9) 0.24239(19) -0.06155(4) 0.0274(2) Uani 1 1 d . . .
H44 H 0.4861 0.2219 -0.0640 0.033 Uiso 1 1 calc R . .
C45 C 0.33847(9) 0.07295(18) -0.07305(4) 0.0274(2) Uani 1 1 d . . .
H45 H 0.3604 -0.0633 -0.0836 0.033 Uiso 1 1 calc R . .
C46 C 0.23181(8) 0.10235(16) -0.06912(3) 0.02107(19) Uani 1 1 d . . .
H46 H 0.1812 -0.0146 -0.0768 0.025 Uiso 1 1 calc R . .
C47 C 0.08292(7) 0.32969(16) -0.04906(3) 0.01678(17) Uani 1 1 d . . .
H47A H 0.0601 0.4850 -0.0551 0.020 Uiso 1 1 calc R . .
H47B H 0.0351 0.2346 -0.0707 0.020 Uiso 1 1 calc R . .
N47 N 0.07187(6) 0.26830(12) -0.00334(2) 0.01386(14) Uani 1 1 d . . .
H47C H 0.1043 0.1356 0.0041 0.021 Uiso 1 1 calc R . .
H47D H 0.0005 0.2588 -0.0024 0.021 Uiso 1 1 calc R . .
H47E H 0.1041 0.3733 0.0160 0.021 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0166(4) 0.0163(4) 0.0159(4) 0.0002(3) 0.0022(3) -0.0017(3)
C2 0.0119(3) 0.0150(4) 0.0159(4) -0.0016(3) 0.0024(3) -0.0006(3)
C3 0.0134(4) 0.0168(4) 0.0186(4) 0.0017(3) 0.0029(3) -0.0002(3)
C4 0.0154(4) 0.0165(4) 0.0221(4) 0.0008(3) 0.0048(3) -0.0024(3)
C5 0.0178(4) 0.0229(5) 0.0257(5) -0.0053(4) 0.0043(3) -0.0055(4)
C6 0.0187(4) 0.0322(5) 0.0239(5) -0.0094(4) 0.0010(4) -0.0062(4)
C7 0.0229(4) 0.0332(5) 0.0177(4) -0.0043(4) -0.0012(3) -0.0018(4)
C8 0.0230(4) 0.0249(5) 0.0166(4) -0.0005(4) 0.0000(3) -0.0027(4)
C9 0.0158(4) 0.0186(4) 0.0165(4) -0.0021(3) 0.0025(3) -0.0005(3)
C10 0.0137(4) 0.0185(4) 0.0201(4) -0.0032(3) 0.0047(3) -0.0013(3)
C11 0.0125(3) 0.0137(4) 0.0138(4) -0.0016(3) 0.0036(3) 0.0003(3)
O12 0.0212(3) 0.0149(3) 0.0158(3) 0.0015(2) 0.0012(2) -0.0035(2)
O13 0.0140(3) 0.0154(3) 0.0143(3) 0.0011(2) 0.0018(2) 0.0003(2)
C21 0.0168(4) 0.0158(4) 0.0152(4) 0.0004(3) 0.0034(3) -0.0007(3)
C22 0.0166(4) 0.0166(4) 0.0146(4) 0.0006(3) 0.0043(3) 0.0008(3)
C23 0.0208(4) 0.0172(4) 0.0162(4) -0.0025(3) 0.0024(3) -0.0016(3)
C24 0.0199(4) 0.0147(4) 0.0208(4) 0.0000(3) 0.0039(3) -0.0018(3)
C25 0.0200(4) 0.0197(4) 0.0216(4) 0.0062(4) 0.0050(3) 0.0015(3)
C26 0.0237(4) 0.0276(5) 0.0178(4) 0.0071(4) 0.0051(3) 0.0040(4)
C27 0.0221(4) 0.0278(5) 0.0149(4) -0.0002(4) 0.0015(3) 0.0029(4)
C28 0.0196(4) 0.0201(4) 0.0166(4) -0.0006(3) 0.0021(3) 0.0003(3)
C29 0.0155(4) 0.0172(4) 0.0147(4) 0.0005(3) 0.0026(3) 0.0010(3)
C30 0.0155(4) 0.0163(4) 0.0175(4) 0.0017(3) 0.0035(3) 0.0019(3)
C31 0.0176(4) 0.0170(4) 0.0155(4) 0.0004(3) 0.0048(3) 0.0007(3)
O32 0.0296(4) 0.0223(3) 0.0147(3) 0.0029(3) 0.0027(3) -0.0083(3)
O33 0.0250(3) 0.0250(4) 0.0151(3) 0.0000(3) 0.0009(3) -0.0039(3)
C41 0.0163(4) 0.0175(4) 0.0128(4) 0.0008(3) 0.0042(3) 0.0016(3)
C42 0.0196(4) 0.0179(4) 0.0174(4) -0.0007(3) 0.0057(3) 0.0003(3)
C43 0.0185(4) 0.0269(5) 0.0246(5) 0.0016(4) 0.0062(3) -0.0026(4)
C44 0.0209(4) 0.0316(5) 0.0332(5) 0.0073(4) 0.0134(4) 0.0071(4)
C45 0.0317(5) 0.0209(5) 0.0342(5) 0.0026(4) 0.0179(4) 0.0075(4)
C46 0.0258(5) 0.0175(4) 0.0217(4) -0.0013(3) 0.0093(4) 0.0001(4)
C47 0.0153(4) 0.0214(4) 0.0134(4) 0.0007(3) 0.0025(3) 0.0008(3)
N47 0.0130(3) 0.0139(3) 0.0149(3) 0.0002(3) 0.0033(3) -0.0007(3)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.3761(12) . ?
C1 C9 1.4207(12) . ?
C2 C3 1.4223(12) . ?
C2 C11 1.5027(12) . ?
C3 C4 1.3721(13) . ?
C4 C10 1.4171(13) . ?
C5 C6 1.3712(15) . ?
C5 C10 1.4230(13) . ?
C6 C7 1.4160(16) . ?
C7 C8 1.3727(14) . ?
C8 C9 1.4185(13) . ?
C9 C10 1.4221(13) . ?
C11 O13 1.2655(11) . ?
C11 O12 1.2666(11) . ?
C21 C22 1.3764(12) . ?
C21 C29 1.4186(12) . ?
C22 C23 1.4188(13) . ?
C22 C31 1.4924(12) . ?
C23 C24 1.3709(13) . ?
C24 C30 1.4223(13) . ?
C25 C26 1.3705(14) . ?
C25 C30 1.4221(13) . ?
C26 C27 1.4135(15) . ?
C27 C28 1.3747(13) . ?
C28 C29 1.4225(13) . ?
C29 C30 1.4248(13) . ?
C31 O33 1.2226(12) . ?
C31 O32 1.3240(11) . ?
C41 C42 1.3929(13) . ?
C41 C46 1.3954(13) . ?
C41 C47 1.5084(12) . ?
C42 C43 1.3935(13) . ?
C43 C44 1.3920(16) . ?
C44 C45 1.3880(17) . ?
C45 C46 1.3895(14) . ?
C47 N47 1.5005(12) . ?

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 C1 C9 120.93(8) . . ?
C1 C2 C3 119.57(8) . . ?
C1 C2 C11 120.62(8) . . ?
C3 C2 C11 119.77(8) . . ?
C4 C3 C2 120.54(8) . . ?
C3 C4 C10 120.88(9) . . ?
C6 C5 C10 120.63(10) . . ?
C5 C6 C7 120.51(9) . . ?
C8 C7 C6 120.17(10) . . ?
C7 C8 C9 120.58(10) . . ?
C8 C9 C1 121.43(9) . . ?
C8 C9 C10 119.38(8) . . ?
C1 C9 C10 119.19(8) . . ?
C4 C10 C9 118.86(8) . . ?
C4 C10 C5 122.41(9) . . ?
C9 C10 C5 118.73(9) . . ?
O13 C11 O12 122.17(8) . . ?
O13 C11 C2 118.52(8) . . ?
O12 C11 C2 119.31(8) . . ?
C22 C21 C29 120.80(8) . . ?
C21 C22 C23 120.09(8) . . ?
C21 C22 C31 120.85(8) . . ?
C23 C22 C31 119.02(8) . . ?
C24 C23 C22 120.40(8) . . ?
C23 C24 C30 120.66(9) . . ?
C26 C25 C30 120.49(9) . . ?
C25 C26 C27 120.69(9) . . ?
C28 C27 C26 120.34(9) . . ?
C27 C28 C29 120.33(9) . . ?
C21 C29 C28 121.78(9) . . ?
C21 C29 C30 118.97(8) . . ?
C28 C29 C30 119.25(8) . . ?
C25 C30 C24 122.03(9) . . ?
C25 C30 C29 118.91(8) . . ?
C24 C30 C29 119.05(8) . . ?
O33 C31 O32 123.64(9) . . ?
O33 C31 C22 123.55(9) . . ?
O32 C31 C22 112.80(8) . . ?
C42 C41 C46 119.41(8) . . ?
C42 C41 C47 120.91(8) . . ?
C46 C41 C47 119.67(8) . . ?
C41 C42 C43 120.06(9) . . ?
C44 C43 C42 120.23(10) . . ?
C45 C44 C43 119.79(9) . . ?
C44 C45 C46 120.08(10) . . ?
C45 C46 C41 120.43(9) . . ?
N47 C47 C41 110.58(7) . . ?

_diffrn_measured_fraction_theta_max 0.895
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.049

#===END