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

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

# Electronic Su_publ_co
ntact_author_name        'Yoshitane Imai'
_publ_contact_author_address     
;
Kinki University
Higashi-osaka
577-8502
JAPAN
;

_publ_contact_author_email       Y-IMAI@APCH.KINDAI.AC.JP

_publ_section_title              
;
Multiple Molecular Response Columnar Host System
Composed of Rac-2-Amino-1,2-diphenylethanol and 1-Fluorenecarboxylic
Acid
;
loop_
_publ_author_name
'Yoshitane Imai'
'Michiya Fujiki'
'Takunori Harada'
'Kakuhiro Kawaguchi'
'Reiko Kuroda'
'Yoshio Matsubara'
;
K.Murata
;
'Keiko Nagasaki'
'Yoko Nakano'
'Tomohiro Sato'

data_imai82_1
_database_code_depnum_ccdc_archive 'CCDC 678709'
#data_im6375a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H31 N O4'
_chemical_formula_weight         469.56
_chemical_absolute_configuration 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           Monoclinic
_symmetry_space_group_name_H-M   C2

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

_cell_length_a                   28.581(2)
_cell_length_b                   6.1600(5)
_cell_length_c                   14.2146(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.4410(10)
_cell_angle_gamma                90.00
_cell_volume                     2481.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5132
_cell_measurement_theta_min      1.44
_cell_measurement_theta_max      27.88

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9676
_exptl_absorpt_correction_T_max  0.9877
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(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       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11038
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         27.88
_reflns_number_total             5573
_reflns_number_gt                5132
_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 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)+(0.0647P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.7(9)
_refine_ls_number_reflns         5573
_refine_ls_number_parameters     328
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1146
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_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 0.12723(6) 0.7633(3) 0.10446(12) 0.0188(4) Uani 1 1 d . . .
C2 C 0.10835(7) 0.9549(3) 0.06403(15) 0.0283(4) Uani 1 1 d . . .
H2 H 0.1239 1.0277 0.0180 0.034 Uiso 1 1 calc R . .
C3 C 0.06692(8) 1.0413(4) 0.09023(17) 0.0360(5) Uani 1 1 d . . .
H3 H 0.0538 1.1690 0.0599 0.043 Uiso 1 1 calc R . .
C4 C 0.04468(7) 0.9440(3) 0.15963(15) 0.0298(4) Uani 1 1 d . . .
H4 H 0.0167 1.0046 0.1779 0.036 Uiso 1 1 calc R . .
C5 C 0.06384(6) 0.7572(3) 0.20203(13) 0.0215(4) Uani 1 1 d . . .
C6 C 0.10476(6) 0.6641(3) 0.17407(12) 0.0178(4) Uani 1 1 d . . .
C7 C 0.06697(7) 0.2694(4) 0.34693(13) 0.0287(4) Uani 1 1 d . . .
H7 H 0.0872 0.1469 0.3566 0.034 Uiso 1 1 calc R . .
C8 C 0.02641(7) 0.2837(4) 0.39181(14) 0.0305(5) Uani 1 1 d . . .
H8 H 0.0188 0.1688 0.4317 0.037 Uiso 1 1 calc R . .
C9 C -0.00279(7) 0.4631(4) 0.37884(13) 0.0294(5) Uani 1 1 d . . .
H9 H -0.0299 0.4710 0.4110 0.035 Uiso 1 1 calc R . .
C10 C 0.00684(6) 0.6308(4) 0.31993(13) 0.0252(4) Uani 1 1 d . . .
H10 H -0.0133 0.7537 0.3111 0.030 Uiso 1 1 calc R . .
C11 C 0.04689(6) 0.6156(3) 0.27356(12) 0.0210(4) Uani 1 1 d . . .
C12 C 0.07698(6) 0.4371(3) 0.28829(12) 0.0219(4) Uani 1 1 d . . .
C13 C 0.11712(6) 0.4585(3) 0.22931(13) 0.0218(4) Uani 1 1 d . . .
C14 C 0.16905(6) 0.6615(3) 0.06663(12) 0.0184(4) Uani 1 1 d . . .
O15 O 0.16721(4) 0.4594(2) 0.05298(8) 0.0192(3) Uani 1 1 d . . .
O16 O 0.20203(4) 0.7822(2) 0.04827(9) 0.0242(3) Uani 1 1 d . . .
C21 C 0.15321(6) 0.7062(3) 0.70547(13) 0.0193(4) Uani 1 1 d . . .
C22 C 0.15041(7) 0.5764(3) 0.62520(14) 0.0258(4) Uani 1 1 d . . .
H22 H 0.1674 0.4436 0.6271 0.031 Uiso 1 1 calc R . .
C23 C 0.12291(7) 0.6395(4) 0.54223(14) 0.0316(5) Uani 1 1 d . . .
H23 H 0.1210 0.5494 0.4876 0.038 Uiso 1 1 calc R . .
C24 C 0.09837(7) 0.8328(4) 0.53862(15) 0.0326(5) Uani 1 1 d . . .
H24 H 0.0796 0.8758 0.4816 0.039 Uiso 1 1 calc R . .
C25 C 0.10110(7) 0.9633(4) 0.61778(15) 0.0328(5) Uani 1 1 d . . .
H25 H 0.0843 1.0967 0.6153 0.039 Uiso 1 1 calc R . .
C26 C 0.12845(6) 0.8998(3) 0.70130(14) 0.0254(4) Uani 1 1 d . . .
H26 H 0.1301 0.9899 0.7559 0.031 Uiso 1 1 calc R . .
C27 C 0.18348(6) 0.6407(3) 0.79626(13) 0.0195(4) Uani 1 1 d . . .
H27 H 0.1658 0.6748 0.8508 0.023 Uiso 1 1 calc R . .
O28 O 0.19495(4) 0.4166(2) 0.79971(9) 0.0236(3) Uani 1 1 d . . .
H28 H 0.1732 0.3467 0.8206 0.035 Uiso 1 1 calc R . .
C29 C 0.25948(6) 0.7357(3) 0.72933(12) 0.0189(4) Uani 1 1 d . . .
C30 C 0.25786(6) 0.8954(3) 0.65964(13) 0.0230(4) Uani 1 1 d . . .
H30 H 0.2405 1.0250 0.6659 0.028 Uiso 1 1 calc R . .
C31 C 0.28135(7) 0.8666(4) 0.58119(14) 0.0290(5) Uani 1 1 d . . .
H31 H 0.2800 0.9763 0.5339 0.035 Uiso 1 1 calc R . .
C32 C 0.30677(7) 0.6786(4) 0.57141(14) 0.0290(5) Uani 1 1 d . . .
H32 H 0.3227 0.6589 0.5174 0.035 Uiso 1 1 calc R . .
C33 C 0.30897(7) 0.5194(4) 0.64058(14) 0.0273(4) Uani 1 1 d . . .
H33 H 0.3268 0.3911 0.6344 0.033 Uiso 1 1 calc R . .
C34 C 0.28519(6) 0.5469(3) 0.71898(13) 0.0221(4) Uani 1 1 d . . .
H34 H 0.2865 0.4363 0.7658 0.026 Uiso 1 1 calc R . .
C35 C 0.23060(6) 0.7658(3) 0.81030(12) 0.0173(3) Uani 1 1 d . . .
H35 H 0.2232 0.9239 0.8147 0.021 Uiso 1 1 calc R . .
N36 N 0.25710(5) 0.6971(2) 0.90300(10) 0.0180(3) Uani 1 1 d . . .
H36A H 0.2661 0.5560 0.8992 0.027 Uiso 1 1 calc R . .
H36B H 0.2382 0.7111 0.9495 0.027 Uiso 1 1 calc R . .
H36C H 0.2831 0.7822 0.9168 0.027 Uiso 1 1 calc R . .
O41 O 0.12182(5) 1.2924(2) 0.88724(10) 0.0279(3) Uani 1 1 d . . .
H41 H 0.1301 1.3437 0.9416 0.042 Uiso 1 1 calc R . .
C42 C 0.07220(8) 1.3147(4) 0.86395(16) 0.0398(6) Uani 1 1 d . . .
H42A H 0.0565 1.1870 0.8883 0.048 Uiso 1 1 calc R . .
H42B H 0.0643 1.3168 0.7941 0.048 Uiso 1 1 calc R . .
C43 C 0.05338(9) 1.5174(5) 0.90432(17) 0.0482(7) Uani 1 1 d . . .
H43A H 0.0607 1.5154 0.9736 0.072 Uiso 1 1 calc R . .
H43B H 0.0191 1.5243 0.8867 0.072 Uiso 1 1 calc R . .
H43C H 0.0681 1.6448 0.8790 0.072 Uiso 1 1 calc R . .
H13A H 0.1471(7) 0.474(4) 0.2737(14) 0.022(5) Uiso 1 1 d . . .
H13B H 0.1182(7) 0.334(4) 0.1892(16) 0.031(6) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.389(2) . ?
C1 C2 1.391(3) . ?
C1 C14 1.509(2) . ?
C2 C3 1.392(3) . ?
C3 C4 1.378(3) . ?
C4 C5 1.379(3) . ?
C5 C6 1.405(3) . ?
C5 C11 1.469(3) . ?
C6 C13 1.508(3) . ?
C7 C12 1.380(3) . ?
C7 C8 1.396(3) . ?
C8 C9 1.383(3) . ?
C9 C10 1.380(3) . ?
C10 C11 1.396(3) . ?
C11 C12 1.395(3) . ?
C12 C13 1.512(2) . ?
C14 O16 1.254(2) . ?
C14 O15 1.260(2) . ?
C21 C26 1.384(3) . ?
C21 C22 1.387(3) . ?
C21 C27 1.513(3) . ?
C22 C23 1.386(3) . ?
C23 C24 1.379(3) . ?
C24 C25 1.377(3) . ?
C25 C26 1.390(3) . ?
C27 O28 1.418(2) . ?
C27 C35 1.542(2) . ?
C29 C30 1.392(3) . ?
C29 C34 1.394(3) . ?
C29 C35 1.512(2) . ?
C30 C31 1.385(3) . ?
C31 C32 1.383(3) . ?
C32 C33 1.384(3) . ?
C33 C34 1.389(3) . ?
C35 N36 1.493(2) . ?
O41 C42 1.421(3) . ?
C42 C43 1.503(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
C6 C1 C2 118.53(17) . . ?
C6 C1 C14 122.09(16) . . ?
C2 C1 C14 119.23(16) . . ?
C1 C2 C3 120.77(19) . . ?
C4 C3 C2 120.83(19) . . ?
C3 C4 C5 118.82(18) . . ?
C4 C5 C6 120.99(18) . . ?
C4 C5 C11 130.57(17) . . ?
C6 C5 C11 108.33(17) . . ?
C1 C6 C5 120.01(17) . . ?
C1 C6 C13 129.94(16) . . ?
C5 C6 C13 110.05(16) . . ?
C12 C7 C8 118.6(2) . . ?
C9 C8 C7 120.8(2) . . ?
C10 C9 C8 120.99(17) . . ?
C9 C10 C11 118.46(19) . . ?
C12 C11 C10 120.62(18) . . ?
C12 C11 C5 108.66(15) . . ?
C10 C11 C5 130.62(18) . . ?
C7 C12 C11 120.56(16) . . ?
C7 C12 C13 129.19(18) . . ?
C11 C12 C13 110.20(16) . . ?
C6 C13 C12 102.64(15) . . ?
O16 C14 O15 124.83(17) . . ?
O16 C14 C1 118.61(16) . . ?
O15 C14 C1 116.51(16) . . ?
C26 C21 C22 119.14(17) . . ?
C26 C21 C27 119.95(17) . . ?
C22 C21 C27 120.90(17) . . ?
C23 C22 C21 120.3(2) . . ?
C24 C23 C22 120.2(2) . . ?
C25 C24 C23 119.92(19) . . ?
C24 C25 C26 120.0(2) . . ?
C21 C26 C25 120.45(19) . . ?
O28 C27 C21 113.16(15) . . ?
O28 C27 C35 106.72(14) . . ?
C21 C27 C35 111.76(14) . . ?
C30 C29 C34 118.93(16) . . ?
C30 C29 C35 118.94(17) . . ?
C34 C29 C35 121.99(16) . . ?
C31 C30 C29 120.48(19) . . ?
C32 C31 C30 120.24(19) . . ?
C31 C32 C33 119.84(18) . . ?
C32 C33 C34 120.1(2) . . ?
C33 C34 C29 120.39(18) . . ?
N36 C35 C29 111.86(14) . . ?
N36 C35 C27 107.90(14) . . ?
C29 C35 C27 113.21(14) . . ?
O41 C42 C43 112.8(2) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        27.88
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.059

#==END

data_imai82_2
_database_code_depnum_ccdc_archive 'CCDC 678710'
#data_im7623a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H33 N O4'
_chemical_formula_weight         483.58

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                   13.9729(15)
_cell_length_b                   6.1709(7)
_cell_length_c                   29.952(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.452(2)
_cell_angle_gamma                90.00
_cell_volume                     2574.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    3968
_cell_measurement_theta_min      1.36
_cell_measurement_theta_max      27.89

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_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             1032
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9641
_exptl_absorpt_correction_T_max  0.9919
_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       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14902
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         27.89
_reflns_number_total             5835
_reflns_number_gt                3968
_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 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)+(0.0721P)²+0.3262P] 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         5835
_refine_ls_number_parameters     329
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0662
_refine_ls_wR_factor_ref         0.1632
_refine_ls_wR_factor_gt          0.1398
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.002
_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 0.00851(18) 0.7365(4) 0.05232(8) 0.0274(6) Uani 1 1 d . . .
H1 H -0.0210 0.8026 0.0261 0.033 Uiso 1 1 calc R . .
C2 C 0.08971(18) 0.8265(4) 0.07440(9) 0.0299(6) Uani 1 1 d . . .
H2 H 0.1165 0.9550 0.0631 0.036 Uiso 1 1 calc R . .
C3 C 0.13242(17) 0.7310(4) 0.11288(8) 0.0239(5) Uani 1 1 d . . .
H3 H 0.1872 0.7974 0.1279 0.029 Uiso 1 1 calc R . .
C4 C 0.09663(15) 0.5395(4) 0.12999(7) 0.0173(5) Uani 1 1 d . . .
C5 C 0.01496(15) 0.4467(4) 0.10753(7) 0.0184(5) Uani 1 1 d . . .
C6 C -0.02911(16) 0.5474(4) 0.06924(8) 0.0209(5) Uani 1 1 d . . .
C7 C -0.17796(18) 0.4432(5) 0.01603(9) 0.0342(7) Uani 1 1 d . . .
H7 H -0.1746 0.5665 -0.0028 0.041 Uiso 1 1 calc R . .
C8 C -0.24808(18) 0.2878(5) 0.00723(10) 0.0396(7) Uani 1 1 d . . .
H8 H -0.2936 0.3051 -0.0178 0.047 Uiso 1 1 calc R . .
C9 C -0.25275(18) 0.1076(5) 0.03437(9) 0.0363(7) Uani 1 1 d . . .
H9 H -0.3010 0.0016 0.0276 0.044 Uiso 1 1 calc R . .
C10 C -0.18756(17) 0.0793(5) 0.07160(9) 0.0316(6) Uani 1 1 d . . .
H10 H -0.1909 -0.0448 0.0902 0.038 Uiso 1 1 calc R . .
C11 C -0.11788(16) 0.2362(4) 0.08088(8) 0.0237(5) Uani 1 1 d . . .
C12 C -0.11237(16) 0.4157(4) 0.05294(8) 0.0235(5) Uani 1 1 d . . .
C13 C -0.03942(16) 0.2449(4) 0.11849(8) 0.0208(5) Uani 1 1 d . . .
H13A H -0.0665 0.2575 0.1480 0.025 Uiso 1 1 calc R . .
H13B H 0.0022 0.1150 0.1185 0.025 Uiso 1 1 calc R . .
C14 C 0.14806(14) 0.4349(4) 0.16994(8) 0.0178(5) Uani 1 1 d . . .
O15 O 0.15947(11) 0.2314(3) 0.16835(5) 0.0211(4) Uani 1 1 d . . .
O16 O 0.17913(11) 0.5508(3) 0.20243(5) 0.0248(4) Uani 1 1 d . . .
C21 C 0.50325(15) 0.4794(4) 0.16118(7) 0.0180(5) Uani 1 1 d . . .
C22 C 0.58194(16) 0.3433(4) 0.16051(8) 0.0243(6) Uani 1 1 d . . .
H22 H 0.5842 0.2140 0.1778 0.029 Uiso 1 1 calc R . .
C23 C 0.65732(17) 0.3938(4) 0.13491(8) 0.0278(6) Uani 1 1 d . . .
H23 H 0.7105 0.2980 0.1344 0.033 Uiso 1 1 calc R . .
C24 C 0.65550(17) 0.5827(4) 0.11015(8) 0.0269(6) Uani 1 1 d . . .
H24 H 0.7072 0.6169 0.0926 0.032 Uiso 1 1 calc R . .
C25 C 0.57816(18) 0.7218(4) 0.11102(9) 0.0302(6) Uani 1 1 d . . .
H25 H 0.5771 0.8531 0.0944 0.036 Uiso 1 1 calc R . .
C26 C 0.50189(17) 0.6694(4) 0.13623(8) 0.0238(5) Uani 1 1 d . . .
H26 H 0.4484 0.7643 0.1364 0.029 Uiso 1 1 calc R . .
C27 C 0.42032(16) 0.4228(4) 0.18886(8) 0.0194(5) Uani 1 1 d . . .
H27 H 0.3594 0.4682 0.1717 0.023 Uiso 1 1 calc R . .
O28 O 0.41425(12) 0.1975(3) 0.19796(5) 0.0243(4) Uani 1 1 d . . .
H28 H 0.3861 0.1344 0.1758 0.036 Uiso 1 1 calc R . .
C29 C 0.52249(15) 0.5053(4) 0.26106(7) 0.0179(5) Uani 1 1 d . . .
C30 C 0.59313(16) 0.6622(4) 0.25909(8) 0.0231(5) Uani 1 1 d . . .
H30 H 0.5796 0.7924 0.2429 0.028 Uiso 1 1 calc R . .
C31 C 0.68399(17) 0.6291(4) 0.28083(8) 0.0278(6) Uani 1 1 d . . .
H31 H 0.7324 0.7363 0.2791 0.033 Uiso 1 1 calc R . .
C32 C 0.70382(16) 0.4412(4) 0.30487(8) 0.0270(6) Uani 1 1 d . . .
H32 H 0.7656 0.4192 0.3197 0.032 Uiso 1 1 calc R . .
C33 C 0.63301(16) 0.2849(4) 0.30715(8) 0.0269(6) Uani 1 1 d . . .
H33 H 0.6462 0.1557 0.3238 0.032 Uiso 1 1 calc R . .
C34 C 0.54269(16) 0.3167(4) 0.28515(8) 0.0233(5) Uani 1 1 d . . .
H34 H 0.4946 0.2086 0.2866 0.028 Uiso 1 1 calc R . .
C35 C 0.42705(15) 0.5410(4) 0.23400(7) 0.0182(5) Uani 1 1 d . . .
H35 H 0.4203 0.6998 0.2279 0.022 Uiso 1 1 calc R . .
N36 N 0.34386(12) 0.4717(3) 0.25920(6) 0.0176(4) Uani 1 1 d . . .
H36A H 0.3530 0.3328 0.2688 0.026 Uiso 1 1 calc R . .
H36B H 0.2888 0.4799 0.2409 0.026 Uiso 1 1 calc R . .
H36C H 0.3392 0.5603 0.2832 0.026 Uiso 1 1 calc R . .
O41 O -0.30485(11) -0.0932(3) -0.11998(5) 0.0249(4) Uani 1 1 d . . .
H41 H -0.2544 -0.1376 -0.1305 0.037 Uiso 1 1 calc R . .
C42 C -0.32318(17) -0.2190(4) -0.08127(8) 0.0255(6) Uani 1 1 d . . .
H42A H -0.2701 -0.2005 -0.0577 0.031 Uiso 1 1 calc R . .
H42B H -0.3278 -0.3745 -0.0892 0.031 Uiso 1 1 calc R . .
C43 C -0.41595(17) -0.1428(4) -0.06435(8) 0.0262(6) Uani 1 1 d . . .
H43A H -0.4661 -0.1398 -0.0896 0.031 Uiso 1 1 calc R . .
H43B H -0.4075 0.0069 -0.0528 0.031 Uiso 1 1 calc R . .
C44 C -0.4494(2) -0.2868(5) -0.02740(9) 0.0379(7) Uani 1 1 d . . .
H44A H -0.4628 -0.4326 -0.0393 0.057 Uiso 1 1 calc R . .
H44B H -0.5078 -0.2259 -0.0163 0.057 Uiso 1 1 calc R . .
H44C H -0.3990 -0.2946 -0.0028 0.057 Uiso 1 1 calc R . .


_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 1.384(3) . ?
C1 C6 1.392(3) . ?
C2 C3 1.388(3) . ?
C3 C4 1.396(3) . ?
C4 C5 1.401(3) . ?
C4 C14 1.494(3) . ?
C5 C6 1.404(3) . ?
C5 C13 1.508(3) . ?
C6 C12 1.471(3) . ?
C7 C8 1.382(4) . ?
C7 C12 1.390(3) . ?
C8 C9 1.382(4) . ?
C9 C10 1.395(4) . ?
C10 C11 1.386(3) . ?
C11 C12 1.394(4) . ?
C11 C13 1.511(3) . ?
C14 O16 1.257(3) . ?
C14 O15 1.267(3) . ?
C21 C22 1.385(3) . ?
C21 C26 1.390(3) . ?
C21 C27 1.517(3) . ?
C22 C23 1.386(3) . ?
C23 C24 1.381(4) . ?
C24 C25 1.382(3) . ?
C25 C26 1.391(3) . ?
C27 O28 1.421(3) . ?
C27 C35 1.533(3) . ?
C29 C30 1.387(3) . ?
C29 C34 1.387(3) . ?
C29 C35 1.522(3) . ?
C30 C31 1.396(3) . ?
C31 C32 1.381(4) . ?
C32 C33 1.388(3) . ?
C33 C34 1.391(3) . ?
C35 N36 1.497(3) . ?
O41 C42 1.435(3) . ?
C42 C43 1.503(3) . ?
C43 C44 1.520(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
C2 C1 C6 118.8(2) . . ?
C1 C2 C3 120.7(2) . . ?
C2 C3 C4 121.4(2) . . ?
C3 C4 C5 118.1(2) . . ?
C3 C4 C14 119.7(2) . . ?
C5 C4 C14 122.1(2) . . ?
C4 C5 C6 120.0(2) . . ?
C4 C5 C13 129.6(2) . . ?
C6 C5 C13 110.29(19) . . ?
C1 C6 C5 121.0(2) . . ?
C1 C6 C12 130.8(2) . . ?
C5 C6 C12 108.2(2) . . ?
C8 C7 C12 118.7(3) . . ?
C7 C8 C9 120.8(2) . . ?
C8 C9 C10 120.9(3) . . ?
C11 C10 C9 118.5(3) . . ?
C10 C11 C12 120.4(2) . . ?
C10 C11 C13 129.2(2) . . ?
C12 C11 C13 110.4(2) . . ?
C7 C12 C11 120.7(2) . . ?
C7 C12 C6 130.7(2) . . ?
C11 C12 C6 108.6(2) . . ?
C5 C13 C11 102.45(19) . . ?
O16 C14 O15 123.8(2) . . ?
O16 C14 C4 119.3(2) . . ?
O15 C14 C4 116.9(2) . . ?
C22 C21 C26 118.8(2) . . ?
C22 C21 C27 120.6(2) . . ?
C26 C21 C27 120.6(2) . . ?
C21 C22 C23 120.7(2) . . ?
C24 C23 C22 120.3(2) . . ?
C23 C24 C25 119.7(2) . . ?
C24 C25 C26 119.9(2) . . ?
C21 C26 C25 120.6(2) . . ?
O28 C27 C21 112.94(19) . . ?
O28 C27 C35 107.29(18) . . ?
C21 C27 C35 112.04(18) . . ?
C30 C29 C34 119.4(2) . . ?
C30 C29 C35 118.3(2) . . ?
C34 C29 C35 122.2(2) . . ?
C29 C30 C31 120.2(2) . . ?
C32 C31 C30 120.3(2) . . ?
C31 C32 C33 119.6(2) . . ?
C32 C33 C34 120.2(2) . . ?
C29 C34 C33 120.3(2) . . ?
N36 C35 C29 111.89(17) . . ?
N36 C35 C27 108.18(17) . . ?
C29 C35 C27 113.08(18) . . ?
O41 C42 C43 108.4(2) . . ?
C42 C43 C44 112.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.949
_diffrn_reflns_theta_full        27.89
_diffrn_measured_fraction_theta_full 0.949
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.090

#==END

data_imai82_3
_database_code_depnum_ccdc_archive 'CCDC 678711'
#data_im7647a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H35 N O4'
_chemical_formula_weight         497.61

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                   16.4950(13)
_cell_length_b                   6.2388(5)
_cell_length_c                   26.400(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.2010(10)
_cell_angle_gamma                90.00
_cell_volume                     2633.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4610
_cell_measurement_theta_min      1.33
_cell_measurement_theta_max      27.93

_exptl_crystal_description       needle
_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    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9602
_exptl_absorpt_correction_T_max  0.9919
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(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       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15731
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.33
_diffrn_reflns_theta_max         27.93
_reflns_number_total             5973
_reflns_number_gt                4610
_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 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)+(0.0493P)²+3.8395P] 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         5973
_refine_ls_number_parameters     338
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0692
_refine_ls_wR_factor_ref         0.1606
_refine_ls_wR_factor_gt          0.1487
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.003
_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 0.91613(19) -0.3522(7) 0.0153(2) 0.104(2) Uani 1 1 d . . .
H1 H 0.9720 -0.3894 0.0153 0.125 Uiso 1 1 calc R . .
C2 C 0.85039(19) -0.4784(7) -0.0107(2) 0.0978(19) Uani 1 1 d . . .
H2 H 0.8612 -0.6026 -0.0288 0.117 Uiso 1 1 calc R . .
C3 C 0.76939(16) -0.4266(5) -0.01068(12) 0.0432(7) Uani 1 1 d . . .
H3 H 0.7249 -0.5175 -0.0279 0.052 Uiso 1 1 calc R . .
C4 C 0.75211(13) -0.2432(3) 0.01416(8) 0.0205(4) Uani 1 1 d . . .
C5 C 0.81890(13) -0.1154(3) 0.04047(8) 0.0201(4) Uani 1 1 d . . .
C6 C 0.90027(15) -0.1736(4) 0.04089(11) 0.0368(6) Uani 1 1 d . . .
C7 C 1.04404(18) -0.0042(6) 0.08325(17) 0.0725(13) Uani 1 1 d . . .
H7 H 1.0758 -0.1116 0.0714 0.087 Uiso 1 1 calc R . .
C8 C 1.08363(16) 0.1661(5) 0.11251(13) 0.0497(8) Uani 1 1 d . . .
H8 H 1.1429 0.1756 0.1208 0.060 Uiso 1 1 calc R . .
C9 C 1.03869(15) 0.3199(4) 0.12950(9) 0.0341(6) Uani 1 1 d . . .
H9 H 1.0666 0.4364 0.1496 0.041 Uiso 1 1 calc R . .
C10 C 0.95260(17) 0.3079(5) 0.11774(12) 0.0488(8) Uani 1 1 d . . .
H10 H 0.9212 0.4170 0.1294 0.059 Uiso 1 1 calc R . .
C11 C 0.91217(14) 0.1375(4) 0.08906(9) 0.0285(5) Uani 1 1 d . . .
C12 C 0.95806(14) -0.0167(4) 0.07145(10) 0.0305(5) Uani 1 1 d . . .
C13 C 0.81998(15) 0.0869(5) 0.07112(12) 0.0404(7) Uani 1 1 d . . .
H13A H 0.7951 0.0642 0.1012 0.049 Uiso 1 1 calc R . .
H13B H 0.7893 0.2032 0.0489 0.049 Uiso 1 1 calc R . .
C14 C 0.66260(13) -0.1839(4) 0.00984(8) 0.0205(4) Uani 1 1 d . . .
O15 O 0.64494(10) 0.0130(3) 0.00558(6) 0.0280(4) Uani 1 1 d . . .
O16 O 0.61041(9) -0.3303(3) 0.00848(6) 0.0270(4) Uani 1 1 d . . .
C21 C 0.49494(12) 0.3418(4) 0.17765(8) 0.0203(4) Uani 1 1 d . . .
C22 C 0.47277(13) 0.1444(4) 0.19381(9) 0.0232(5) Uani 1 1 d . . .
H22 H 0.4548 0.0337 0.1689 0.028 Uiso 1 1 calc R . .
C23 C 0.47642(14) 0.1061(4) 0.24602(9) 0.0267(5) Uani 1 1 d . . .
H23 H 0.4612 -0.0303 0.2568 0.032 Uiso 1 1 calc R . .
C24 C 0.50216(14) 0.2667(4) 0.28236(9) 0.0291(5) Uani 1 1 d . . .
H24 H 0.5046 0.2413 0.3182 0.035 Uiso 1 1 calc R . .
C25 C 0.52436(15) 0.4640(4) 0.26656(9) 0.0318(5) Uani 1 1 d . . .
H25 H 0.5421 0.5746 0.2916 0.038 Uiso 1 1 calc R . .
C26 C 0.52090(14) 0.5020(4) 0.21439(9) 0.0274(5) Uani 1 1 d . . .
H26 H 0.5364 0.6384 0.2038 0.033 Uiso 1 1 calc R . .
C27 C 0.49135(13) 0.3791(4) 0.12046(8) 0.0211(4) Uani 1 1 d . . .
H27 H 0.4353 0.3317 0.0993 0.025 Uiso 1 1 calc R . .
O28 O 0.50329(10) 0.5955(3) 0.10833(6) 0.0271(4) Uani 1 1 d . . .
H28 H 0.4577 0.6615 0.1036 0.041 Uiso 1 1 calc R . .
C29 C 0.64668(13) 0.2876(4) 0.13657(8) 0.0211(4) Uani 1 1 d . . .
C30 C 0.68581(14) 0.1314(4) 0.17156(9) 0.0283(5) Uani 1 1 d . . .
H30 H 0.6584 -0.0012 0.1735 0.034 Uiso 1 1 calc R . .
C31 C 0.76482(14) 0.1677(5) 0.20378(9) 0.0340(6) Uani 1 1 d . . .
H31 H 0.7911 0.0604 0.2278 0.041 Uiso 1 1 calc R . .
C32 C 0.80494(14) 0.3589(4) 0.20100(9) 0.0307(5) Uani 1 1 d . . .
H32 H 0.8590 0.3835 0.2231 0.037 Uiso 1 1 calc R . .
C33 C 0.76691(14) 0.5153(4) 0.16623(9) 0.0284(5) Uani 1 1 d . . .
H33 H 0.7949 0.6470 0.1643 0.034 Uiso 1 1 calc R . .
C34 C 0.68786(13) 0.4801(4) 0.13409(9) 0.0240(5) Uani 1 1 d . . .
H34 H 0.6618 0.5881 0.1103 0.029 Uiso 1 1 calc R . .
C35 C 0.55918(13) 0.2463(4) 0.10371(8) 0.0207(4) Uani 1 1 d . . .
H35 H 0.5463 0.0912 0.1073 0.025 Uiso 1 1 calc R . .
N36 N 0.55357(10) 0.2895(3) 0.04742(7) 0.0197(4) Uani 1 1 d . . .
H36A H 0.5758 0.4207 0.0440 0.030 Uiso 1 1 calc R . .
H36B H 0.4990 0.2869 0.0293 0.030 Uiso 1 1 calc R . .
H36C H 0.5825 0.1872 0.0346 0.030 Uiso 1 1 calc R . .
O41 O 0.35761(10) 0.8207(3) 0.08931(6) 0.0301(4) Uani 1 1 d . . .
H41 H 0.3541 0.8710 0.0593 0.045 Uiso 1 1 calc R . .
C41 C 0.29015(14) 0.8998(4) 0.10891(9) 0.0283(5) Uani 1 1 d . . .
H41A H 0.2366 0.8752 0.0828 0.034 Uiso 1 1 calc R . .
H41B H 0.2968 1.0561 0.1150 0.034 Uiso 1 1 calc R . .
C42 C 0.28817(16) 0.7884(4) 0.15928(10) 0.0338(6) Uani 1 1 d . . .
H42A H 0.3429 0.8094 0.1845 0.041 Uiso 1 1 calc R . .
H42B H 0.2450 0.8575 0.1740 0.041 Uiso 1 1 calc R . .
C43 C 0.27018(17) 0.5521(4) 0.15388(11) 0.0385(6) Uani 1 1 d . . .
H43A H 0.3134 0.4815 0.1395 0.046 Uiso 1 1 calc R . .
H43B H 0.2154 0.5297 0.1288 0.046 Uiso 1 1 calc R . .
C44 C 0.26874(19) 0.4484(5) 0.20599(12) 0.0462(7) Uani 1 1 d . . .
H44A H 0.3234 0.4666 0.2306 0.069 Uiso 1 1 calc R . .
H44B H 0.2564 0.2952 0.2007 0.069 Uiso 1 1 calc R . .
H44C H 0.2255 0.5167 0.2202 0.069 Uiso 1 1 calc R . .


_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 C6 1.362(4) . ?
C1 C2 1.378(4) . ?
C2 C3 1.375(4) . ?
C3 C4 1.383(3) . ?
C4 C5 1.399(3) . ?
C4 C14 1.499(3) . ?
C5 C6 1.388(3) . ?
C5 C13 1.497(3) . ?
C6 C12 1.463(3) . ?
C7 C12 1.378(4) . ?
C7 C8 1.380(4) . ?
C8 C9 1.354(4) . ?
C9 C10 1.379(4) . ?
C10 C11 1.379(3) . ?
C11 C12 1.374(3) . ?
C11 C13 1.511(3) . ?
C14 O16 1.250(3) . ?
C14 O15 1.261(3) . ?
C21 C22 1.382(3) . ?
C21 C26 1.385(3) . ?
C21 C27 1.514(3) . ?
C22 C23 1.386(3) . ?
C23 C24 1.380(3) . ?
C24 C25 1.378(4) . ?
C25 C26 1.385(3) . ?
C27 O28 1.412(3) . ?
C27 C35 1.542(3) . ?
C29 C30 1.388(3) . ?
C29 C34 1.389(3) . ?
C29 C35 1.513(3) . ?
C30 C31 1.389(3) . ?
C31 C32 1.375(4) . ?
C32 C33 1.380(3) . ?
C33 C34 1.388(3) . ?
C35 N36 1.491(3) . ?
O41 C41 1.425(3) . ?
C41 C42 1.508(3) . ?
C42 C43 1.504(4) . ?
C43 C44 1.526(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
C6 C1 C2 119.4(3) . . ?
C3 C2 C1 120.8(3) . . ?
C2 C3 C4 120.5(2) . . ?
C3 C4 C5 118.6(2) . . ?
C3 C4 C14 118.8(2) . . ?
C5 C4 C14 122.55(19) . . ?
C6 C5 C4 119.8(2) . . ?
C6 C5 C13 109.5(2) . . ?
C4 C5 C13 130.7(2) . . ?
C1 C6 C5 120.9(2) . . ?
C1 C6 C12 130.0(2) . . ?
C5 C6 C12 109.1(2) . . ?
C12 C7 C8 119.3(3) . . ?
C9 C8 C7 120.6(2) . . ?
C8 C9 C10 120.3(2) . . ?
C11 C10 C9 119.9(3) . . ?
C12 C11 C10 119.6(2) . . ?
C12 C11 C13 110.1(2) . . ?
C10 C11 C13 130.3(2) . . ?
C11 C12 C7 120.4(2) . . ?
C11 C12 C6 108.5(2) . . ?
C7 C12 C6 131.2(2) . . ?
C5 C13 C11 102.90(19) . . ?
O16 C14 O15 124.5(2) . . ?
O16 C14 C4 118.71(19) . . ?
O15 C14 C4 116.68(19) . . ?
C22 C21 C26 119.1(2) . . ?
C22 C21 C27 119.74(19) . . ?
C26 C21 C27 121.1(2) . . ?
C21 C22 C23 120.7(2) . . ?
C24 C23 C22 119.8(2) . . ?
C25 C24 C23 119.8(2) . . ?
C24 C25 C26 120.3(2) . . ?
C25 C26 C21 120.2(2) . . ?
O28 C27 C21 113.54(18) . . ?
O28 C27 C35 107.30(17) . . ?
C21 C27 C35 110.48(17) . . ?
C30 C29 C34 119.0(2) . . ?
C30 C29 C35 119.0(2) . . ?
C34 C29 C35 121.96(19) . . ?
C29 C30 C31 120.4(2) . . ?
C32 C31 C30 120.0(2) . . ?
C31 C32 C33 120.2(2) . . ?
C32 C33 C34 120.0(2) . . ?
C33 C34 C29 120.3(2) . . ?
N36 C35 C29 110.98(17) . . ?
N36 C35 C27 108.47(16) . . ?
C29 C35 C27 113.65(18) . . ?
O41 C41 C42 110.4(2) . . ?
C43 C42 C41 114.5(2) . . ?
C42 C43 C44 112.1(2) . . ?

_diffrn_measured_fraction_theta_max 0.946
_diffrn_reflns_theta_full        27.93
_diffrn_measured_fraction_theta_full 0.946
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.058

#==END


