Electronic Supplementary Material for CrystEngComm
This Journal is © The Royal Society of Chemistry 2003

data_global

_journal_coden_Cambridge         1350

loop_
_publ_author_name
'Asao Nakamura'
'Reiko Kuroda'
'T. Sato'

_publ_contact_author_name        'Dr Asao Nakamura'
_publ_contact_author_address     
;
Kuroda Chiromorphology Project
Japan Science and Technology Corporation
4-7-6 Komaba, Meguro-ku
Tokyo
153-0041
JAPAN
;

_publ_contact_author_email       ASAO@CHIROMOR2.ERATO.RCAST.U-TOKYO.AC.JP

_publ_requested_journal          'Cryst Eng. Comm.'

_publ_section_title              
;
Novel Layered Structures of the Crystals Based on
C-Methylcalix[4]resorcinarene Formed at High Temperature
;

data_nakamura5
_database_code_CSD               214039

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C55 H52 N2 O8'
_chemical_formula_weight         868.99

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                   13.1315(10)
_cell_length_b                   14.2151(11)
_cell_length_c                   14.6358(11)
_cell_angle_alpha                109.4280(10)
_cell_angle_beta                 112.9800(10)
_cell_angle_gamma                97.464(2)
_cell_volume                     2263.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    116(2)
_cell_measurement_reflns_used    14259
_cell_measurement_theta_min      1.59
_cell_measurement_theta_max      28.31

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             920
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      116(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            14259
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         28.31
_reflns_number_total             9980
_reflns_number_gt                7009
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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^)+(0.0510P)^2^+0.0000P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9980
_refine_ls_number_parameters     625
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0952
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_restrained_S_all      0.933
_refine_ls_shift/su_max          0.257
_refine_ls_shift/su_mean         0.003

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 0.19460(11) 0.00594(10) -0.07844(10) 0.0211(3) Uani 1 1 d . . .
H1 H 0.1433 0.0370 -0.0598 0.025 Uiso 1 1 calc R . .
C2 C 0.20923(11) 0.01323(10) -0.16502(10) 0.0207(3) Uani 1 1 d . . .
C3 C 0.28688(11) -0.03401(10) -0.19104(10) 0.0213(3) Uani 1 1 d . . .
C4 C 0.34824(11) -0.08383(10) -0.13127(10) 0.0220(3) Uani 1 1 d . . .
H4 H 0.4002 -0.1143 -0.1494 0.026 Uiso 1 1 calc R . .
C5 C 0.33209(11) -0.08806(10) -0.04493(10) 0.0210(3) Uani 1 1 d . . .
C6 C 0.25237(11) -0.04523(10) -0.01809(10) 0.0207(3) Uani 1 1 d . . .
C7 C 0.23287(11) -0.05134(10) 0.07623(10) 0.0212(3) Uani 1 1 d . . .
H7 H 0.2732 -0.0993 0.0987 0.025 Uiso 1 1 calc R . .
C8 C 0.10553(12) -0.09806(11) 0.04095(11) 0.0283(3) Uani 1 1 d . . .
H8A H 0.0967 -0.0989 0.1028 0.042 Uiso 1 1 calc R . .
H8B H 0.0779 -0.1682 -0.0144 0.042 Uiso 1 1 calc R . .
H8C H 0.0616 -0.0566 0.0122 0.042 Uiso 1 1 calc R . .
O9 O 0.30247(9) -0.02706(7) -0.27680(7) 0.0253(2) Uani 1 1 d . . .
O10 O 0.39702(8) -0.13063(7) 0.02057(7) 0.0252(2) Uani 1 1 d . . .
C11 C 0.15253(11) 0.25061(10) -0.10067(10) 0.0204(3) Uani 1 1 d . . .
H11 H 0.0829 0.2160 -0.1077 0.025 Uiso 1 1 calc R . .
C12 C 0.19771(11) 0.35739(10) -0.03657(10) 0.0196(3) Uani 1 1 d . . .
C13 C 0.30251(11) 0.40780(10) -0.02675(10) 0.0212(3) Uani 1 1 d . . .
C14 C 0.35732(11) 0.35250(11) -0.07988(10) 0.0228(3) Uani 1 1 d . . .
H14 H 0.4265 0.3873 -0.0736 0.027 Uiso 1 1 calc R . .
C15 C 0.30968(11) 0.24563(10) -0.14239(10) 0.0217(3) Uani 1 1 d . . .
C16 C 0.20478(11) 0.19209(10) -0.15501(10) 0.0200(3) Uani 1 1 d . . .
C17 C 0.14964(11) 0.07502(10) -0.22533(10) 0.0208(3) Uani 1 1 d . . .
H17 H 0.1634 0.0595 -0.2892 0.025 Uiso 1 1 calc R . .
C18 C 0.01826(11) 0.04000(11) -0.26866(11) 0.0257(3) Uani 1 1 d . . .
H18A H -0.0135 -0.0309 -0.3230 0.039 Uiso 1 1 calc R . .
H18B H -0.0154 0.0844 -0.3007 0.039 Uiso 1 1 calc R . .
H18C H 0.0012 0.0445 -0.2095 0.039 Uiso 1 1 calc R . .
O19 O 0.35629(8) 0.51358(7) 0.03334(8) 0.0269(2) Uani 1 1 d . . .
O20 O 0.37138(9) 0.19765(8) -0.19041(8) 0.0288(2) Uani 1 1 d . . .
C21 C 0.17894(11) 0.36136(10) 0.17621(10) 0.0205(3) Uani 1 1 d . . .
H21 H 0.1368 0.2934 0.1237 0.025 Uiso 1 1 calc R . .
C22 C 0.22639(11) 0.37924(10) 0.28600(10) 0.0202(3) Uani 1 1 d . . .
C23 C 0.29184(11) 0.48056(10) 0.36231(10) 0.0214(3) Uani 1 1 d . . .
C24 C 0.30720(11) 0.56089(10) 0.33129(10) 0.0223(3) Uani 1 1 d . . .
H24 H 0.3514 0.6283 0.3840 0.027 Uiso 1 1 calc R . .
C25 C 0.25655(11) 0.54054(10) 0.22141(11) 0.0211(3) Uani 1 1 d . . .
C26 C 0.19123(11) 0.43945(10) 0.14124(10) 0.0196(3) Uani 1 1 d . . .
C27 C 0.13630(11) 0.41748(10) 0.02037(10) 0.0205(3) Uani 1 1 d . . .
H27 H 0.1481 0.4855 0.0170 0.025 Uiso 1 1 calc R . .
C28 C 0.00504(11) 0.36597(11) -0.03659(11) 0.0253(3) Uani 1 1 d . . .
H28A H -0.0270 0.3557 -0.1116 0.038 Uiso 1 1 calc R . .
H28B H -0.0296 0.4103 -0.0006 0.038 Uiso 1 1 calc R . .
H28C H -0.0106 0.2996 -0.0332 0.038 Uiso 1 1 calc R . .
O29 O 0.34416(9) 0.49755(8) 0.47163(7) 0.0266(2) Uani 1 1 d . . .
O30 O 0.27244(8) 0.61790(7) 0.18781(8) 0.0259(2) Uani 1 1 d . . .
C31 C 0.22718(11) 0.12014(10) 0.20326(10) 0.0205(3) Uani 1 1 d . . .
H31 H 0.1469 0.0976 0.1617 0.025 Uiso 1 1 calc R . .
C32 C 0.28928(11) 0.05414(10) 0.17400(10) 0.0203(3) Uani 1 1 d . . .
C33 C 0.40904(11) 0.08910(10) 0.23846(10) 0.0213(3) Uani 1 1 d . . .
C34 C 0.46372(11) 0.18621(10) 0.32596(10) 0.0230(3) Uani 1 1 d . . .
H34 H 0.5439 0.2088 0.3676 0.028 Uiso 1 1 calc R . .
C35 C 0.39851(11) 0.24948(10) 0.35117(10) 0.0217(3) Uani 1 1 d . . .
C36 C 0.27834(11) 0.21808(10) 0.29123(10) 0.0206(3) Uani 1 1 d . . .
C37 C 0.20998(11) 0.29082(10) 0.32096(11) 0.0225(3) Uani 1 1 d . . .
H37 H 0.2448 0.3231 0.4010 0.027 Uiso 1 1 calc R . .
C38 C 0.08222(12) 0.23676(11) 0.27845(12) 0.0294(3) Uani 1 1 d . . .
H38A H 0.0435 0.2080 0.2000 0.044 Uiso 1 1 calc R . .
H38B H 0.0474 0.2866 0.3069 0.044 Uiso 1 1 calc R . .
H38C H 0.0754 0.1816 0.3017 0.044 Uiso 1 1 calc R . .
O39 O 0.47867(8) 0.02713(8) 0.22286(8) 0.0262(2) Uani 1 1 d . . .
O40 O 0.45923(8) 0.34528(7) 0.43921(7) 0.0273(2) Uani 1 1 d . . .
C41 C 0.67172(14) 0.98704(12) 0.53333(12) 0.0341(4) Uani 1 1 d . . .
C42 C 0.61859(16) 1.01231(12) 0.59998(13) 0.0436(4) Uani 1 1 d . . .
H42 H 0.5709 0.9597 0.6023 0.052 Uiso 1 1 calc R . .
C43 C 0.63689(15) 1.11549(12) 0.66256(12) 0.0395(4) Uani 1 1 d . . .
H43 H 0.6012 1.1308 0.7072 0.047 Uiso 1 1 calc R . .
N44 N 0.70309(11) 1.19447(9) 0.66241(10) 0.0329(3) Uani 1 1 d . . .
C45 C 0.75296(13) 1.17060(12) 0.59718(12) 0.0343(4) Uani 1 1 d . . .
H45 H 0.7991 1.2252 0.5960 0.041 Uiso 1 1 calc R . .
C46 C 0.73999(13) 1.06964(12) 0.53154(12) 0.0344(4) Uani 1 1 d . . .
H46 H 0.7760 1.0569 0.4870 0.041 Uiso 1 1 calc R . .
C47 C 0.65199(15) 0.87929(12) 0.46786(12) 0.0383(4) Uani 1 1 d . . .
C48 C 0.62983(14) 0.78745(12) 0.41537(12) 0.0357(4) Uani 1 1 d . . .
C49 C 0.60721(13) 0.68269(12) 0.35500(12) 0.0327(4) Uani 1 1 d . . .
C50 C 0.58747(13) 0.59139(12) 0.30215(12) 0.0298(3) Uani 1 1 d . . .
C51 C 0.57185(12) 0.48533(11) 0.23490(11) 0.0256(3) Uani 1 1 d . . .
C52 C 0.64494(12) 0.46451(11) 0.18834(11) 0.0276(3) Uani 1 1 d . . .
H52 H 0.7047 0.5185 0.2019 0.033 Uiso 1 1 calc R . .
C53 C 0.62798(12) 0.36315(11) 0.12204(11) 0.0270(3) Uani 1 1 d . . .
H53 H 0.6773 0.3506 0.0909 0.032 Uiso 1 1 calc R . .
N54 N 0.54485(10) 0.28153(9) 0.09959(9) 0.0245(3) Uani 1 1 d . . .
C55 C 0.47453(12) 0.30197(11) 0.14443(11) 0.0264(3) Uani 1 1 d . . .
H55 H 0.4154 0.2463 0.1291 0.032 Uiso 1 1 calc R . .
C56 C 0.48465(12) 0.40100(11) 0.21230(11) 0.0265(3) Uani 1 1 d . . .
H56 H 0.4342 0.4113 0.2424 0.032 Uiso 1 1 calc R . .
C61 C 1.10731(12) 0.65050(12) 0.52431(12) 0.0330(4) Uani 1 1 d . . .
C62 C 1.06960(12) 0.57110(12) 0.42154(12) 0.0329(4) Uani 1 1 d . . .
H62 H 1.0978 0.5138 0.4157 0.039 Uiso 1 1 calc R . .
C63 C 0.99083(12) 0.57487(11) 0.32718(11) 0.0279(3) Uani 1 1 d . . .
C64 C 0.94884(12) 0.66021(11) 0.33726(11) 0.0284(3) Uani 1 1 d . . .
H64 H 0.8964 0.6638 0.2746 0.034 Uiso 1 1 calc R . .
C65 C 0.98324(13) 0.74065(12) 0.43886(12) 0.0305(3) Uani 1 1 d . . .
C66 C 1.06299(13) 0.73455(12) 0.53112(12) 0.0324(4) Uani 1 1 d . . .
H66 H 1.0874 0.7883 0.5995 0.039 Uiso 1 1 calc R . .
C67 C 1.19189(15) 0.64372(15) 0.62547(13) 0.0487(5) Uani 1 1 d . . .
H67A H 1.2021 0.7010 0.6892 0.073 Uiso 1 1 calc R . .
H67B H 1.2651 0.6468 0.6249 0.073 Uiso 1 1 calc R . .
H67C H 1.1624 0.5789 0.6267 0.073 Uiso 1 1 calc R . .
C68 C 0.95221(13) 0.48779(12) 0.21667(12) 0.0374(4) Uani 1 1 d . . .
H68A H 1.0174 0.4847 0.2024 0.056 Uiso 1 1 calc R . .
H68B H 0.8941 0.5006 0.1614 0.056 Uiso 1 1 calc R . .
H68C H 0.9205 0.4225 0.2158 0.056 Uiso 1 1 calc R . .
C69 C 0.93372(15) 0.83097(13) 0.44808(13) 0.0444(4) Uani 1 1 d . . .
H69A H 0.8798 0.8217 0.3765 0.067 Uiso 1 1 calc R . .
H69B H 0.9953 0.8949 0.4819 0.067 Uiso 1 1 calc R . .
H69C H 0.8945 0.8340 0.4918 0.067 Uiso 1 1 calc R . .
H30 H 0.2855(15) 0.6808(15) 0.2449(15) 0.067(6) Uiso 1 1 d . . .
H39 H 0.4448(14) -0.0284(13) 0.1541(14) 0.049(5) Uiso 1 1 d . . .
H19 H 0.3247(14) 0.5405(13) 0.0777(14) 0.047(5) Uiso 1 1 d . . .
H9 H 0.3696(16) -0.0407(14) -0.2709(14) 0.060(6) Uiso 1 1 d . . .
H29 H 0.4001(16) 0.5550(15) 0.5056(15) 0.059(6) Uiso 1 1 d . . .
H20 H 0.3365(15) 0.1275(14) -0.2260(14) 0.052(5) Uiso 1 1 d . . .
H10 H 0.4325(16) -0.1703(15) -0.0154(15) 0.066(6) Uiso 1 1 d . . .
H40 H 0.4146(16) 0.3828(16) 0.4562(16) 0.070(6) Uiso 1 1 d . . .

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 0.0206(7) 0.0165(7) 0.0238(7) 0.0053(6) 0.0102(6) 0.0068(6)
C2 0.0214(7) 0.0153(7) 0.0198(6) 0.0044(6) 0.0070(6) 0.0048(5)
C3 0.0236(7) 0.0187(7) 0.0196(6) 0.0061(6) 0.0101(6) 0.0050(6)
C4 0.0234(7) 0.0186(7) 0.0247(7) 0.0068(6) 0.0127(6) 0.0094(6)
C5 0.0234(7) 0.0149(7) 0.0214(7) 0.0066(6) 0.0080(6) 0.0070(6)
C6 0.0222(7) 0.0152(7) 0.0214(7) 0.0053(6) 0.0093(6) 0.0041(6)
C7 0.0237(7) 0.0175(7) 0.0241(7) 0.0091(6) 0.0120(6) 0.0079(6)
C8 0.0303(8) 0.0207(7) 0.0299(8) 0.0065(6) 0.0148(6) 0.0035(6)
O9 0.0293(6) 0.0300(6) 0.0244(5) 0.0140(4) 0.0158(4) 0.0153(5)
O10 0.0326(6) 0.0233(5) 0.0249(5) 0.0116(4) 0.0145(4) 0.0159(5)
C11 0.0187(7) 0.0218(7) 0.0204(6) 0.0102(6) 0.0072(5) 0.0073(6)
C12 0.0218(7) 0.0194(7) 0.0179(6) 0.0095(6) 0.0073(5) 0.0088(6)
C13 0.0237(7) 0.0184(7) 0.0193(6) 0.0094(6) 0.0068(6) 0.0060(6)
C14 0.0209(7) 0.0267(8) 0.0243(7) 0.0141(6) 0.0107(6) 0.0074(6)
C15 0.0249(7) 0.0246(8) 0.0214(7) 0.0124(6) 0.0123(6) 0.0124(6)
C16 0.0225(7) 0.0196(7) 0.0185(6) 0.0094(6) 0.0080(6) 0.0092(6)
C17 0.0228(7) 0.0198(7) 0.0199(6) 0.0070(6) 0.0102(6) 0.0088(6)
C18 0.0256(8) 0.0222(7) 0.0244(7) 0.0078(6) 0.0084(6) 0.0076(6)
O19 0.0291(6) 0.0187(5) 0.0306(5) 0.0068(4) 0.0155(5) 0.0044(4)
O20 0.0312(6) 0.0256(6) 0.0361(6) 0.0115(5) 0.0220(5) 0.0119(5)
C21 0.0184(7) 0.0166(7) 0.0235(7) 0.0045(6) 0.0099(6) 0.0056(5)
C22 0.0192(7) 0.0188(7) 0.0243(7) 0.0080(6) 0.0121(6) 0.0075(6)
C23 0.0211(7) 0.0223(7) 0.0208(6) 0.0076(6) 0.0102(6) 0.0089(6)
C24 0.0226(7) 0.0153(7) 0.0232(7) 0.0032(6) 0.0094(6) 0.0048(6)
C25 0.0204(7) 0.0190(7) 0.0272(7) 0.0104(6) 0.0125(6) 0.0095(6)
C26 0.0175(7) 0.0190(7) 0.0233(7) 0.0079(6) 0.0103(6) 0.0084(6)
C27 0.0221(7) 0.0159(7) 0.0230(7) 0.0082(6) 0.0093(6) 0.0076(6)
C28 0.0239(7) 0.0232(8) 0.0273(7) 0.0095(6) 0.0103(6) 0.0106(6)
O29 0.0324(6) 0.0206(5) 0.0209(5) 0.0063(4) 0.0096(4) 0.0049(5)
O30 0.0332(6) 0.0157(5) 0.0258(5) 0.0076(4) 0.0120(4) 0.0067(4)
C31 0.0208(7) 0.0203(7) 0.0209(6) 0.0107(6) 0.0087(6) 0.0050(6)
C32 0.0250(7) 0.0179(7) 0.0202(6) 0.0098(6) 0.0113(6) 0.0059(6)
C33 0.0267(7) 0.0220(7) 0.0226(7) 0.0138(6) 0.0138(6) 0.0109(6)
C34 0.0195(7) 0.0251(7) 0.0227(7) 0.0123(6) 0.0068(6) 0.0049(6)
C35 0.0286(8) 0.0163(7) 0.0183(6) 0.0075(6) 0.0096(6) 0.0039(6)
C36 0.0253(7) 0.0187(7) 0.0207(6) 0.0109(6) 0.0111(6) 0.0071(6)
C37 0.0268(7) 0.0193(7) 0.0214(7) 0.0071(6) 0.0127(6) 0.0057(6)
C38 0.0320(8) 0.0233(8) 0.0369(8) 0.0109(7) 0.0214(7) 0.0081(6)
O39 0.0246(5) 0.0270(6) 0.0257(5) 0.0086(5) 0.0114(4) 0.0114(4)
O40 0.0268(6) 0.0199(5) 0.0244(5) 0.0038(4) 0.0072(4) 0.0039(4)
C41 0.0521(10) 0.0247(8) 0.0245(7) 0.0103(7) 0.0153(7) 0.0168(7)
C42 0.0816(13) 0.0207(8) 0.0346(9) 0.0125(7) 0.0336(9) 0.0092(8)
C43 0.0676(12) 0.0274(9) 0.0325(8) 0.0132(7) 0.0311(8) 0.0141(8)
N44 0.0453(8) 0.0214(7) 0.0298(7) 0.0100(6) 0.0159(6) 0.0105(6)
C45 0.0359(9) 0.0265(8) 0.0380(9) 0.0123(7) 0.0168(7) 0.0063(7)
C46 0.0348(9) 0.0356(9) 0.0312(8) 0.0115(7) 0.0150(7) 0.0131(7)
C47 0.0567(11) 0.0290(9) 0.0292(8) 0.0119(7) 0.0190(8) 0.0166(8)
C48 0.0496(10) 0.0290(9) 0.0307(8) 0.0125(7) 0.0191(7) 0.0172(8)
C49 0.0435(9) 0.0266(9) 0.0298(8) 0.0106(7) 0.0184(7) 0.0145(7)
C50 0.0365(9) 0.0277(8) 0.0298(8) 0.0131(7) 0.0172(7) 0.0147(7)
C51 0.0310(8) 0.0231(8) 0.0237(7) 0.0114(6) 0.0109(6) 0.0130(6)
C52 0.0298(8) 0.0227(8) 0.0330(8) 0.0132(7) 0.0155(7) 0.0089(6)
C53 0.0306(8) 0.0273(8) 0.0308(8) 0.0145(7) 0.0174(7) 0.0151(7)
N54 0.0283(7) 0.0227(6) 0.0258(6) 0.0130(5) 0.0116(5) 0.0128(5)
C55 0.0275(8) 0.0249(8) 0.0292(7) 0.0150(6) 0.0120(6) 0.0096(6)
C56 0.0301(8) 0.0281(8) 0.0282(7) 0.0141(7) 0.0165(6) 0.0144(7)
C61 0.0276(8) 0.0416(9) 0.0294(8) 0.0158(7) 0.0126(7) 0.0083(7)
C62 0.0291(8) 0.0372(9) 0.0374(8) 0.0177(8) 0.0169(7) 0.0149(7)
C63 0.0244(8) 0.0311(8) 0.0286(7) 0.0103(7) 0.0148(6) 0.0069(6)
C64 0.0277(8) 0.0336(8) 0.0254(7) 0.0140(7) 0.0124(6) 0.0090(7)
C65 0.0356(9) 0.0302(8) 0.0296(8) 0.0130(7) 0.0185(7) 0.0092(7)
C66 0.0347(9) 0.0327(9) 0.0247(7) 0.0082(7) 0.0137(7) 0.0047(7)
C67 0.0434(10) 0.0593(12) 0.0361(9) 0.0214(9) 0.0101(8) 0.0168(9)
C68 0.0385(9) 0.0408(10) 0.0322(8) 0.0112(8) 0.0179(7) 0.0157(8)
C69 0.0622(12) 0.0378(10) 0.0341(9) 0.0144(8) 0.0220(8) 0.0209(9)

_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 1.3877(19) . ?
C1 C6 1.3902(18) . ?
C2 C3 1.3953(17) . ?
C2 C17 1.5224(18) . ?
C3 O9 1.3801(16) . ?
C3 C4 1.3879(18) . ?
C4 C5 1.3790(19) . ?
C5 O10 1.3762(15) . ?
C5 C6 1.3958(17) . ?
C6 C7 1.5260(18) . ?
C7 C32 1.5169(17) . ?
C7 C8 1.5209(18) . ?
C11 C12 1.3857(18) . ?
C11 C16 1.3891(17) . ?
C12 C13 1.3960(18) . ?
C12 C27 1.5181(17) . ?
C13 O19 1.3758(16) . ?
C13 C14 1.3849(18) . ?
C14 C15 1.3849(19) . ?
C15 O20 1.3729(15) . ?
C15 C16 1.3951(18) . ?
C16 C17 1.5227(18) . ?
C17 C18 1.5293(18) . ?
C21 C26 1.3843(18) . ?
C21 C22 1.3930(18) . ?
C22 C23 1.3853(18) . ?
C22 C37 1.5270(19) . ?
C23 C24 1.3810(19) . ?
C23 O29 1.3899(15) . ?
C24 C25 1.3849(18) . ?
C25 O30 1.3692(16) . ?
C25 C26 1.3963(18) . ?
C26 C27 1.5247(17) . ?
C27 C28 1.5317(18) . ?
C31 C32 1.3901(17) . ?
C31 C36 1.3916(17) . ?
C32 C33 1.3917(18) . ?
C33 O39 1.3793(15) . ?
C33 C34 1.3819(18) . ?
C34 C35 1.3799(18) . ?
C35 O40 1.3780(15) . ?
C35 C36 1.3909(18) . ?
C36 C37 1.5203(17) . ?
C37 C38 1.5245(18) . ?
C41 C42 1.389(2) . ?
C41 C46 1.396(2) . ?
C41 C47 1.435(2) . ?
C42 C43 1.375(2) . ?
C43 N44 1.329(2) . ?
N44 C45 1.3362(19) . ?
C45 C46 1.379(2) . ?
C47 C48 1.200(2) . ?
C48 C49 1.375(2) . ?
C49 C50 1.199(2) . ?
C50 C51 1.435(2) . ?
C51 C52 1.3869(19) . ?
C51 C56 1.393(2) . ?
C52 C53 1.3729(19) . ?
C53 N54 1.3353(18) . ?
N54 C55 1.3355(17) . ?
C55 C56 1.3800(19) . ?
C61 C66 1.387(2) . ?
C61 C62 1.388(2) . ?
C61 C67 1.508(2) . ?
C62 C63 1.389(2) . ?
C63 C64 1.3841(19) . ?
C63 C68 1.5066(19) . ?
C64 C65 1.3903(19) . ?
C65 C66 1.387(2) . ?
C65 C69 1.503(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 C6 123.65(12) . . ?
C1 C2 C3 116.87(12) . . ?
C1 C2 C17 122.25(11) . . ?
C3 C2 C17 120.78(12) . . ?
O9 C3 C4 121.26(12) . . ?
O9 C3 C2 117.44(12) . . ?
C4 C3 C2 121.27(12) . . ?
C5 C4 C3 119.90(12) . . ?
O10 C5 C4 121.41(11) . . ?
O10 C5 C6 117.54(12) . . ?
C4 C5 C6 121.00(12) . . ?
C1 C6 C5 117.24(12) . . ?
C1 C6 C7 121.60(11) . . ?
C5 C6 C7 121.13(12) . . ?
C32 C7 C8 113.68(11) . . ?
C32 C7 C6 110.49(11) . . ?
C8 C7 C6 112.06(11) . . ?
C12 C11 C16 124.08(13) . . ?
C11 C12 C13 117.02(12) . . ?
C11 C12 C27 121.78(12) . . ?
C13 C12 C27 121.19(11) . . ?
O19 C13 C14 116.16(12) . . ?
O19 C13 C12 123.06(11) . . ?
C14 C13 C12 120.78(12) . . ?
C15 C14 C13 120.33(13) . . ?
O20 C15 C14 115.94(12) . . ?
O20 C15 C16 123.19(12) . . ?
C14 C15 C16 120.87(12) . . ?
C11 C16 C15 116.90(12) . . ?
C11 C16 C17 121.40(12) . . ?
C15 C16 C17 121.70(11) . . ?
C2 C17 C16 110.85(10) . . ?
C2 C17 C18 111.93(11) . . ?
C16 C17 C18 113.18(10) . . ?
C26 C21 C22 123.41(12) . . ?
C23 C22 C21 117.01(13) . . ?
C23 C22 C37 121.31(12) . . ?
C21 C22 C37 121.66(12) . . ?
C24 C23 C22 121.63(12) . . ?
C24 C23 O29 121.25(12) . . ?
C22 C23 O29 117.10(12) . . ?
C23 C24 C25 119.72(12) . . ?
O30 C25 C24 121.16(12) . . ?
O30 C25 C26 117.94(12) . . ?
C24 C25 C26 120.86(13) . . ?
C21 C26 C25 117.36(12) . . ?
C21 C26 C27 122.05(11) . . ?
C25 C26 C27 120.59(12) . . ?
C12 C27 C26 111.41(10) . . ?
C12 C27 C28 113.37(10) . . ?
C26 C27 C28 111.76(11) . . ?
C32 C31 C36 123.68(12) . . ?
C31 C32 C33 117.03(12) . . ?
C31 C32 C7 123.23(12) . . ?
C33 C32 C7 119.74(11) . . ?
O39 C33 C34 116.38(11) . . ?
O39 C33 C32 122.22(11) . . ?
C34 C33 C32 121.30(12) . . ?
C35 C34 C33 119.58(12) . . ?
O40 C35 C34 116.19(12) . . ?
O40 C35 C36 121.99(12) . . ?
C34 C35 C36 121.82(12) . . ?
C35 C36 C31 116.58(12) . . ?
C35 C36 C37 120.09(11) . . ?
C31 C36 C37 123.30(12) . . ?
C36 C37 C38 114.70(11) . . ?
C36 C37 C22 109.62(11) . . ?
C38 C37 C22 111.87(11) . . ?
C42 C41 C46 117.36(14) . . ?
C42 C41 C47 119.50(15) . . ?
C46 C41 C47 123.12(15) . . ?
C43 C42 C41 119.71(16) . . ?
N44 C43 C42 123.23(15) . . ?
C43 N44 C45 117.29(13) . . ?
N44 C45 C46 123.79(15) . . ?
C45 C46 C41 118.61(15) . . ?
C48 C47 C41 175.42(19) . . ?
C47 C48 C49 178.43(19) . . ?
C50 C49 C48 179.84(19) . . ?
C49 C50 C51 174.10(17) . . ?
C52 C51 C56 117.70(13) . . ?
C52 C51 C50 119.36(14) . . ?
C56 C51 C50 122.93(13) . . ?
C53 C52 C51 119.14(14) . . ?
N54 C53 C52 123.87(13) . . ?
C53 N54 C55 116.78(12) . . ?
N54 C55 C56 123.70(14) . . ?
C55 C56 C51 118.79(13) . . ?
C66 C61 C62 118.09(14) . . ?
C66 C61 C67 121.28(14) . . ?
C62 C61 C67 120.61(14) . . ?
C61 C62 C63 121.78(14) . . ?
C64 C63 C62 118.44(13) . . ?
C64 C63 C68 121.03(13) . . ?
C62 C63 C68 120.53(13) . . ?
C63 C64 C65 121.52(14) . . ?
C66 C65 C64 118.31(14) . . ?
C66 C65 C69 121.09(13) . . ?
C64 C65 C69 120.59(13) . . ?
C61 C66 C65 121.85(14) . . ?

_diffrn_measured_fraction_theta_max 0.886
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.886
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.041

#===END

data_nakamura6
_database_code_CSD               214038

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H60 N2 O8'
_chemical_formula_weight         961.12

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                   17.4271(11)
_cell_length_b                   13.5493(8)
_cell_length_c                   21.6050(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.172(2)
_cell_angle_gamma                90.00
_cell_volume                     5080.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    116(2)
_cell_measurement_reflns_used    31544
_cell_measurement_theta_min      1.44
_cell_measurement_theta_max      28.33

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2040
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      116(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            31544
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_sigmaI/netI    0.1548
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         28.33
_reflns_number_total             11801
_reflns_number_gt                5279
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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^)+(0.0206P)^2^+0.0000P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11801
_refine_ls_number_parameters     689
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.0836
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   0.717
_refine_ls_restrained_S_all      0.717
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.004

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 0.03102(11) 0.14037(13) 0.25254(10) 0.0219(5) Uani 1 1 d . . .
H1 H -0.0127 0.1353 0.2741 0.026 Uiso 1 1 calc R . .
C2 C 0.02065(11) 0.15698(14) 0.18881(10) 0.0199(5) Uani 1 1 d . . .
C3 C 0.08651(11) 0.16380(14) 0.15778(10) 0.0213(5) Uani 1 1 d . . .
C4 C 0.15903(11) 0.15674(13) 0.18908(10) 0.0221(5) Uani 1 1 d . . .
H4 H 0.2026 0.1633 0.1675 0.027 Uiso 1 1 calc R . .
C5 C 0.16678(11) 0.13995(14) 0.25240(10) 0.0215(5) Uani 1 1 d . . .
C6 C 0.10266(11) 0.13086(13) 0.28623(10) 0.0194(5) Uani 1 1 d . . .
C7 C 0.11086(11) 0.10867(14) 0.35557(9) 0.0230(5) Uani 1 1 d . . .
H7 H 0.1540 0.1486 0.3739 0.028 Uiso 1 1 calc R . .
C8 C 0.04031(11) 0.13786(14) 0.38862(10) 0.0309(6) Uani 1 1 d . . .
H8A H 0.0290 0.2064 0.3812 0.046 Uiso 1 1 calc R . .
H8B H 0.0506 0.1268 0.4325 0.046 Uiso 1 1 calc R . .
H8C H -0.0031 0.0987 0.3730 0.046 Uiso 1 1 calc R . .
O9 O 0.08425(8) 0.17919(10) 0.09397(7) 0.0264(4) Uani 1 1 d . . .
O10 O 0.24169(8) 0.13350(10) 0.27992(7) 0.0271(4) Uani 1 1 d . . .
C11 C -0.10217(10) -0.01356(14) 0.15081(10) 0.0226(5) Uani 1 1 d . . .
H11 H -0.1010 -0.0110 0.1939 0.027 Uiso 1 1 calc R . .
C12 C -0.12404(10) -0.10207(14) 0.12121(10) 0.0201(5) Uani 1 1 d . . .
C13 C -0.12496(11) -0.10249(15) 0.05684(10) 0.0220(5) Uani 1 1 d . . .
C14 C -0.10337(11) -0.02156(14) 0.02383(10) 0.0242(5) Uani 1 1 d . . .
H14 H -0.1033 -0.0248 -0.0192 0.029 Uiso 1 1 calc R . .
C15 C -0.08175(11) 0.06479(15) 0.05536(10) 0.0234(5) Uani 1 1 d . . .
C16 C -0.08204(10) 0.07084(14) 0.11975(10) 0.0204(5) Uani 1 1 d . . .
C17 C -0.05930(10) 0.16611(14) 0.15404(10) 0.0230(5) Uani 1 1 d . . .
H17 H -0.0556 0.2171 0.1223 0.028 Uiso 1 1 calc R . .
C18 C -0.12166(11) 0.20031(14) 0.19513(10) 0.0314(6) Uani 1 1 d . . .
H18A H -0.1689 0.2119 0.1697 0.047 Uiso 1 1 calc R . .
H18B H -0.1054 0.2602 0.2161 0.047 Uiso 1 1 calc R . .
H18C H -0.1297 0.1502 0.2253 0.047 Uiso 1 1 calc R . .
O19 O -0.14508(8) -0.19072(11) 0.02647(7) 0.0282(4) Uani 1 1 d . . .
O20 O -0.05606(8) 0.14584(11) 0.02492(8) 0.0281(4) Uani 1 1 d . . .
C21 C -0.05351(11) -0.22857(13) 0.25762(9) 0.0205(5) Uani 1 1 d . . .
H21 H -0.0893 -0.1978 0.2806 0.025 Uiso 1 1 calc R . .
C22 C 0.01367(11) -0.26522(14) 0.28924(10) 0.0202(5) Uani 1 1 d . . .
C23 C 0.06514(11) -0.31310(14) 0.25379(10) 0.0216(5) Uani 1 1 d . . .
C24 C 0.05111(11) -0.32178(14) 0.19022(10) 0.0232(5) Uani 1 1 d . . .
H24 H 0.0861 -0.3545 0.1674 0.028 Uiso 1 1 calc R . .
C25 C -0.01532(11) -0.28163(14) 0.16042(10) 0.0214(5) Uani 1 1 d . . .
C26 C -0.07013(11) -0.23556(14) 0.19316(10) 0.0206(5) Uani 1 1 d . . .
C27 C -0.14301(10) -0.19283(14) 0.15857(9) 0.0221(5) Uani 1 1 d . . .
H27 H -0.1628 -0.2429 0.1285 0.026 Uiso 1 1 calc R . .
C28 C -0.20723(10) -0.17180(15) 0.20063(10) 0.0296(6) Uani 1 1 d . . .
H28A H -0.1915 -0.1195 0.2290 0.044 Uiso 1 1 calc R . .
H28B H -0.2174 -0.2302 0.2237 0.044 Uiso 1 1 calc R . .
H28C H -0.2531 -0.1525 0.1756 0.044 Uiso 1 1 calc R . .
O29 O 0.13139(9) -0.35111(11) 0.28540(7) 0.0283(4) Uani 1 1 d . . .
O30 O -0.02259(9) -0.29006(10) 0.09667(7) 0.0285(4) Uani 1 1 d . . .
C31 C 0.07957(11) -0.07487(14) 0.35817(9) 0.0214(5) Uani 1 1 d . . .
H31 H 0.0294 -0.0586 0.3434 0.026 Uiso 1 1 calc R . .
C32 C 0.13281(11) 0.00102(14) 0.36759(9) 0.0205(5) Uani 1 1 d . . .
C33 C 0.20797(11) -0.02545(15) 0.38884(9) 0.0229(5) Uani 1 1 d . . .
C34 C 0.22805(11) -0.12332(14) 0.39996(9) 0.0245(5) Uani 1 1 d . . .
H34 H 0.2785 -0.1398 0.4137 0.029 Uiso 1 1 calc R . .
C35 C 0.17288(11) -0.19605(15) 0.39059(9) 0.0223(5) Uani 1 1 d . . .
C36 C 0.09669(11) -0.17347(14) 0.36952(9) 0.0209(5) Uani 1 1 d . . .
C37 C 0.03406(10) -0.25238(14) 0.35840(9) 0.0224(5) Uani 1 1 d . . .
H37 H 0.0566 -0.3148 0.3740 0.027 Uiso 1 1 calc R . .
C38 C -0.03440(10) -0.23116(14) 0.39548(9) 0.0287(5) Uani 1 1 d . . .
H38A H -0.0563 -0.1683 0.3833 0.043 Uiso 1 1 calc R . .
H38B H -0.0175 -0.2300 0.4390 0.043 Uiso 1 1 calc R . .
H38C H -0.0725 -0.2818 0.3875 0.043 Uiso 1 1 calc R . .
O39 O 0.26230(8) 0.04861(10) 0.39548(7) 0.0283(4) Uani 1 1 d . . .
O40 O 0.19683(8) -0.29200(11) 0.40275(7) 0.0290(4) Uani 1 1 d . . .
C41 C 0.23513(12) 0.88177(14) 0.18971(10) 0.0239(5) Uani 1 1 d . . .
C42 C 0.15900(12) 0.90521(14) 0.19647(10) 0.0268(5) Uani 1 1 d . . .
H42 H 0.1441 0.9266 0.2345 0.032 Uiso 1 1 calc R . .
C43 C 0.10536(12) 0.89613(14) 0.14532(11) 0.0284(6) Uani 1 1 d . . .
H43 H 0.0545 0.9131 0.1501 0.034 Uiso 1 1 calc R . .
N44 N 0.12240(10) 0.86452(12) 0.08993(8) 0.0278(4) Uani 1 1 d . . .
C45 C 0.19614(12) 0.84026(15) 0.08463(10) 0.0331(6) Uani 1 1 d . . .
H45 H 0.2092 0.8169 0.0465 0.040 Uiso 1 1 calc R . .
C46 C 0.25350(12) 0.84797(15) 0.13229(10) 0.0322(6) Uani 1 1 d . . .
H46 H 0.3039 0.8308 0.1262 0.039 Uiso 1 1 calc R . .
C47 C 0.29457(12) 0.89321(14) 0.23947(10) 0.0274(5) Uani 1 1 d . . .
C48 C 0.34703(12) 0.90154(14) 0.27884(11) 0.0275(5) Uani 1 1 d . . .
C49 C 0.40735(12) 0.91196(14) 0.32400(10) 0.0273(5) Uani 1 1 d . . .
C50 C 0.46032(12) 0.92116(14) 0.36239(11) 0.0280(5) Uani 1 1 d . . .
C51 C 0.52220(11) 0.93424(14) 0.41057(10) 0.0228(5) Uani 1 1 d . . .
C52 C 0.58262(11) 0.99940(14) 0.40288(10) 0.0259(5) Uani 1 1 d . . .
H52 H 0.5857 1.0325 0.3655 0.031 Uiso 1 1 calc R . .
C53 C 0.63760(11) 1.01360(15) 0.45202(10) 0.0279(5) Uani 1 1 d . . .
H53 H 0.6769 1.0586 0.4472 0.034 Uiso 1 1 calc R . .
N54 N 0.63740(9) 0.96627(12) 0.50613(8) 0.0251(4) Uani 1 1 d . . .
C55 C 0.58087(11) 0.90170(14) 0.51222(10) 0.0251(5) Uani 1 1 d . . .
H55 H 0.5812 0.8665 0.5492 0.030 Uiso 1 1 calc R . .
C56 C 0.52204(11) 0.88450(14) 0.46662(10) 0.0241(5) Uani 1 1 d . . .
H56 H 0.4828 0.8402 0.4733 0.029 Uiso 1 1 calc R . .
C61 C 0.69468(12) 0.42369(17) 0.07291(11) 0.0338(6) Uani 1 1 d . . .
C62 C 0.72208(12) 0.42553(17) 0.13510(12) 0.0393(6) Uani 1 1 d . . .
H62 H 0.7417 0.3683 0.1543 0.047 Uiso 1 1 calc R . .
C63 C 0.72041(13) 0.51224(18) 0.16875(11) 0.0442(7) Uani 1 1 d . . .
H63 H 0.7388 0.5130 0.2105 0.053 Uiso 1 1 calc R . .
C64 C 0.69163(12) 0.59755(17) 0.14060(11) 0.0388(6) Uani 1 1 d . . .
H64 H 0.6914 0.6557 0.1635 0.047 Uiso 1 1 calc R . .
C65 C 0.66319(11) 0.59776(17) 0.07883(11) 0.0306(6) Uani 1 1 d . . .
C66 C 0.66458(11) 0.50990(16) 0.04613(11) 0.0325(6) Uani 1 1 d . . .
H66 H 0.6446 0.5088 0.0047 0.039 Uiso 1 1 calc R . .
C67 C 0.70016(13) 0.33069(16) 0.03512(11) 0.0513(7) Uani 1 1 d . . .
H67A H 0.6493 0.3060 0.0233 0.077 Uiso 1 1 calc R . .
H67B H 0.7291 0.2819 0.0595 0.077 Uiso 1 1 calc R . .
H67C H 0.7255 0.3450 -0.0015 0.077 Uiso 1 1 calc R . .
C68 C 0.63577(13) 0.69217(16) 0.04758(11) 0.0488(7) Uani 1 1 d . . .
H68A H 0.6780 0.7237 0.0298 0.073 Uiso 1 1 calc R . .
H68B H 0.6161 0.7353 0.0776 0.073 Uiso 1 1 calc R . .
H68C H 0.5958 0.6778 0.0154 0.073 Uiso 1 1 calc R . .
C71 C 0.63983(15) 0.99621(17) 0.06398(13) 0.0448(7) Uani 1 1 d . . .
C72 C 0.69274(15) 1.04733(18) 0.10365(14) 0.0546(8) Uani 1 1 d . . .
H72 H 0.7382 1.0702 0.0893 0.066 Uiso 1 1 calc R . .
C73 C 0.67760(15) 1.06441(18) 0.16516(14) 0.0552(8) Uani 1 1 d . . .
H73 H 0.7129 1.0993 0.1916 0.066 Uiso 1 1 calc R . .
C74 C 0.60991(15) 1.02937(18) 0.18708(13) 0.0534(8) Uani 1 1 d . . .
H74 H 0.6001 1.0407 0.2281 0.064 Uiso 1 1 calc R . .
C75 C 0.55791(14) 0.97830(17) 0.14818(13) 0.0422(7) Uani 1 1 d . . .
C76 C 0.57357(15) 0.96348(17) 0.08610(14) 0.0554(8) Uani 1 1 d . . .
H76 H 0.5376 0.9303 0.0593 0.066 Uiso 1 1 calc R . .
C77 C 0.65889(16) 0.9805(2) -0.00155(13) 0.0820(10) Uani 1 1 d . . .
H77A H 0.7003 0.9338 -0.0020 0.123 Uiso 1 1 calc R . .
H77B H 0.6742 1.0420 -0.0187 0.123 Uiso 1 1 calc R . .
H77C H 0.6144 0.9554 -0.0260 0.123 Uiso 1 1 calc R . .
C78 C 0.48467(14) 0.94013(18) 0.16937(14) 0.0726(10) Uani 1 1 d . . .
H78A H 0.4959 0.8902 0.2004 0.109 Uiso 1 1 calc R . .
H78B H 0.4537 0.9124 0.1347 0.109 Uiso 1 1 calc R . .
H78C H 0.4571 0.9932 0.1867 0.109 Uiso 1 1 calc R . .
H9 H 0.0371(12) 0.1744(15) 0.0761(10) 0.055(8) Uiso 1 1 d . . .
H39 H 0.3003(12) 0.0362(15) 0.4277(11) 0.060(8) Uiso 1 1 d . . .
H20 H -0.0690(13) 0.1410(16) -0.0144(11) 0.058(9) Uiso 1 1 d . . .
H30 H -0.0656(12) -0.2647(15) 0.0785(11) 0.055(8) Uiso 1 1 d . . .
H19 H -0.1395(12) -0.1865(17) -0.0128(11) 0.060(9) Uiso 1 1 d . . .
H10 H 0.2456(12) 0.1122(16) 0.3203(11) 0.063(9) Uiso 1 1 d . . .
H29 H 0.1664(13) -0.3644(17) 0.2630(12) 0.070(10) Uiso 1 1 d . . .
H40 H 0.1738(13) -0.3349(16) 0.3770(11) 0.069(10) Uiso 1 1 d . . .

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 0.0234(12) 0.0208(11) 0.0220(13) -0.0021(10) 0.0042(10) -0.0001(9)
C2 0.0203(11) 0.0192(11) 0.0197(13) 0.0002(10) -0.0014(10) -0.0015(9)
C3 0.0297(13) 0.0184(11) 0.0156(13) -0.0003(10) 0.0006(10) -0.0021(10)
C4 0.0205(11) 0.0228(12) 0.0236(13) 0.0013(10) 0.0050(10) -0.0044(9)
C5 0.0200(12) 0.0224(12) 0.0211(13) -0.0010(10) -0.0035(10) -0.0032(9)
C6 0.0223(12) 0.0162(11) 0.0195(13) 0.0012(10) 0.0003(10) -0.0008(9)
C7 0.0196(11) 0.0289(12) 0.0199(13) -0.0033(11) -0.0016(10) -0.0043(9)
C8 0.0356(13) 0.0339(13) 0.0234(14) -0.0013(11) 0.0044(11) 0.0041(11)
O9 0.0252(9) 0.0341(9) 0.0193(9) 0.0018(8) -0.0017(8) -0.0050(7)
O10 0.0194(8) 0.0384(9) 0.0227(10) 0.0043(8) -0.0022(7) -0.0034(7)
C11 0.0162(11) 0.0345(13) 0.0166(13) -0.0012(11) -0.0019(10) 0.0037(10)
C12 0.0169(11) 0.0232(12) 0.0198(13) 0.0001(10) -0.0004(10) -0.0009(9)
C13 0.0200(12) 0.0236(12) 0.0216(13) -0.0029(11) -0.0026(10) -0.0007(9)
C14 0.0269(12) 0.0291(12) 0.0159(13) 0.0023(11) -0.0017(10) -0.0025(10)
C15 0.0212(12) 0.0246(12) 0.0238(14) 0.0068(11) -0.0019(10) 0.0000(10)
C16 0.0181(11) 0.0231(12) 0.0193(13) 0.0007(10) -0.0032(10) 0.0001(9)
C17 0.0212(11) 0.0241(12) 0.0229(13) -0.0003(10) -0.0024(10) -0.0001(9)
C18 0.0256(12) 0.0340(13) 0.0333(15) -0.0039(12) -0.0051(11) 0.0047(10)
O19 0.0366(9) 0.0291(9) 0.0184(10) -0.0028(8) -0.0010(8) -0.0060(7)
O20 0.0325(9) 0.0302(9) 0.0199(10) 0.0069(8) -0.0067(8) -0.0065(7)
C21 0.0211(12) 0.0185(11) 0.0230(13) -0.0010(10) 0.0074(10) -0.0029(9)
C22 0.0220(12) 0.0202(11) 0.0188(13) 0.0018(10) 0.0037(10) -0.0036(9)
C23 0.0211(12) 0.0180(11) 0.0254(14) -0.0001(11) -0.0002(10) -0.0018(9)
C24 0.0253(12) 0.0230(12) 0.0221(13) -0.0042(11) 0.0055(10) 0.0012(10)
C25 0.0274(12) 0.0222(12) 0.0146(13) -0.0012(10) 0.0011(10) -0.0052(10)
C26 0.0229(12) 0.0200(11) 0.0192(13) 0.0015(10) 0.0030(10) -0.0033(9)
C27 0.0216(12) 0.0241(12) 0.0205(13) -0.0005(10) 0.0017(10) -0.0038(9)
C28 0.0257(12) 0.0335(13) 0.0296(14) 0.0044(12) 0.0020(11) -0.0029(10)
O29 0.0257(9) 0.0352(9) 0.0241(10) -0.0004(8) 0.0021(8) 0.0073(7)
O30 0.0312(10) 0.0342(9) 0.0196(10) -0.0024(8) -0.0009(8) 0.0045(8)
C31 0.0166(11) 0.0323(13) 0.0152(12) -0.0014(10) 0.0003(9) 0.0013(10)
C32 0.0217(12) 0.0279(12) 0.0118(12) -0.0005(10) 0.0014(10) 0.0007(10)
C33 0.0223(12) 0.0324(13) 0.0138(12) -0.0004(11) 0.0004(10) -0.0056(10)
C34 0.0175(11) 0.0370(13) 0.0185(13) 0.0030(11) -0.0008(10) 0.0012(10)
C35 0.0244(12) 0.0278(12) 0.0151(12) 0.0033(10) 0.0036(10) 0.0041(10)
C36 0.0213(12) 0.0273(12) 0.0143(12) -0.0005(10) 0.0023(10) -0.0004(9)
C37 0.0188(12) 0.0278(12) 0.0207(13) 0.0008(11) 0.0024(10) -0.0006(9)
C38 0.0266(12) 0.0398(14) 0.0198(13) -0.0019(11) 0.0030(11) -0.0067(10)
O39 0.0208(8) 0.0368(9) 0.0256(10) 0.0056(8) -0.0067(8) -0.0063(7)
O40 0.0307(9) 0.0284(9) 0.0278(10) 0.0027(8) 0.0012(8) 0.0045(8)
C41 0.0288(13) 0.0212(12) 0.0208(13) 0.0013(10) -0.0031(11) -0.0016(10)
C42 0.0322(13) 0.0256(12) 0.0228(14) -0.0015(11) 0.0037(11) -0.0035(10)
C43 0.0256(13) 0.0259(12) 0.0340(15) 0.0013(12) 0.0040(12) -0.0037(10)
N44 0.0296(11) 0.0281(11) 0.0250(12) 0.0022(9) -0.0010(9) -0.0035(9)
C45 0.0391(14) 0.0386(14) 0.0218(14) -0.0028(12) 0.0035(12) -0.0007(12)
C46 0.0291(13) 0.0382(14) 0.0280(15) -0.0013(12) -0.0036(12) 0.0042(11)
C47 0.0321(13) 0.0253(13) 0.0245(14) 0.0010(11) 0.0011(12) -0.0008(10)
C48 0.0313(13) 0.0250(12) 0.0255(14) 0.0020(11) -0.0007(11) -0.0015(10)
C49 0.0335(14) 0.0247(13) 0.0230(14) 0.0003(11) -0.0002(12) -0.0010(10)
C50 0.0311(13) 0.0258(13) 0.0267(14) 0.0011(11) 0.0007(12) 0.0017(11)
C51 0.0240(12) 0.0222(12) 0.0221(13) -0.0053(11) 0.0007(10) 0.0035(10)
C52 0.0240(12) 0.0319(13) 0.0219(14) 0.0044(11) 0.0024(11) 0.0055(10)
C53 0.0207(12) 0.0313(13) 0.0318(15) 0.0040(12) 0.0023(11) -0.0006(10)
N54 0.0199(10) 0.0312(11) 0.0242(12) 0.0020(9) 0.0018(9) 0.0001(8)
C55 0.0249(12) 0.0292(13) 0.0215(13) 0.0052(11) 0.0035(11) 0.0037(10)
C56 0.0220(12) 0.0229(12) 0.0274(14) -0.0021(11) 0.0021(11) -0.0009(9)
C61 0.0324(14) 0.0420(15) 0.0284(15) -0.0014(13) 0.0110(12) -0.0065(12)
C62 0.0396(15) 0.0425(15) 0.0361(17) 0.0103(14) 0.0047(13) -0.0008(12)
C63 0.0531(17) 0.0559(17) 0.0224(15) 0.0032(14) -0.0035(13) -0.0138(14)
C64 0.0499(16) 0.0389(15) 0.0285(16) -0.0038(13) 0.0073(13) -0.0120(12)
C65 0.0246(13) 0.0423(15) 0.0260(15) 0.0010(13) 0.0082(11) -0.0006(11)
C66 0.0254(13) 0.0518(16) 0.0207(14) -0.0003(13) 0.0051(11) -0.0032(12)
C67 0.0580(17) 0.0501(16) 0.0491(18) -0.0053(15) 0.0229(15) -0.0052(13)
C68 0.0503(16) 0.0568(17) 0.0412(18) 0.0070(15) 0.0145(14) 0.0074(13)
C71 0.0455(17) 0.0406(16) 0.0493(19) -0.0047(15) 0.0104(15) 0.0044(13)
C72 0.0448(17) 0.0542(18) 0.066(2) 0.0109(17) 0.0085(17) 0.0128(14)
C73 0.0517(19) 0.0571(18) 0.055(2) 0.0097(17) -0.0071(16) 0.0088(15)
C74 0.0529(19) 0.0524(18) 0.055(2) 0.0046(16) 0.0050(16) 0.0114(15)
C75 0.0462(17) 0.0327(15) 0.0501(19) 0.0010(14) 0.0179(15) 0.0053(12)
C76 0.0555(19) 0.0425(16) 0.070(2) -0.0062(16) 0.0174(17) 0.0012(14)
C77 0.098(2) 0.090(2) 0.064(2) -0.016(2) 0.037(2) -0.0021(19)
C78 0.067(2) 0.0523(18) 0.102(3) 0.0089(18) 0.0301(19) 0.0015(16)

_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 1.391(3) . ?
C1 C6 1.393(2) . ?
C2 C3 1.384(3) . ?
C2 C17 1.527(2) . ?
C3 C4 1.382(2) . ?
C3 O9 1.391(2) . ?
C4 C5 1.381(3) . ?
C5 O10 1.388(2) . ?
C5 C6 1.395(3) . ?
C6 C7 1.522(3) . ?
C7 C32 1.524(2) . ?
C7 C8 1.529(2) . ?
C11 C16 1.387(2) . ?
C11 C12 1.396(2) . ?
C12 C13 1.389(3) . ?
C12 C27 1.523(2) . ?
C13 C14 1.379(3) . ?
C13 O19 1.393(2) . ?
C14 C15 1.389(2) . ?
C15 O20 1.376(2) . ?
C15 C16 1.394(3) . ?
C16 C17 1.523(2) . ?
C17 C18 1.536(2) . ?
C21 C22 1.393(2) . ?
C21 C26 1.400(3) . ?
C22 C23 1.391(3) . ?
C22 C37 1.515(3) . ?
C23 C24 1.378(3) . ?
C23 O29 1.386(2) . ?
C24 C25 1.384(3) . ?
C25 O30 1.376(2) . ?
C25 C26 1.387(3) . ?
C26 C27 1.528(2) . ?
C27 C28 1.531(2) . ?
C31 C36 1.386(2) . ?
C31 C32 1.388(2) . ?
C32 C33 1.395(2) . ?
C33 O39 1.378(2) . ?
C33 C34 1.387(2) . ?
C34 C35 1.379(2) . ?
C35 O40 1.383(2) . ?
C35 C36 1.398(2) . ?
C36 C37 1.531(2) . ?
C37 C38 1.523(2) . ?
C41 C42 1.385(2) . ?
C41 C46 1.387(3) . ?
C41 C47 1.433(3) . ?
C42 C43 1.387(3) . ?
C43 N44 1.330(3) . ?
N44 C45 1.341(2) . ?
C45 C46 1.373(3) . ?
C47 C48 1.197(3) . ?
C48 C49 1.376(3) . ?
C49 C50 1.191(3) . ?
C50 C51 1.441(3) . ?
C51 C56 1.386(3) . ?
C51 C52 1.395(3) . ?
C52 C53 1.378(3) . ?
C53 N54 1.334(2) . ?
N54 C55 1.333(2) . ?
C55 C56 1.376(3) . ?
C61 C62 1.385(3) . ?
C61 C66 1.386(3) . ?
C61 C67 1.509(3) . ?
C62 C63 1.383(3) . ?
C63 C64 1.379(3) . ?
C64 C65 1.381(3) . ?
C65 C66 1.386(3) . ?
C65 C68 1.504(3) . ?
C71 C76 1.363(3) . ?
C71 C72 1.386(3) . ?
C71 C77 1.498(3) . ?
C72 C73 1.397(3) . ?
C73 C74 1.394(3) . ?
C74 C75 1.367(3) . ?
C75 C76 1.407(3) . ?
C75 C78 1.487(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
C2 C1 C6 124.22(19) . . ?
C3 C2 C1 116.82(18) . . ?
C3 C2 C17 121.07(19) . . ?
C1 C2 C17 122.10(18) . . ?
C4 C3 C2 121.4(2) . . ?
C4 C3 O9 115.98(18) . . ?
C2 C3 O9 122.66(18) . . ?
C3 C4 C5 119.96(19) . . ?
C4 C5 O10 116.03(18) . . ?
C4 C5 C6 121.48(19) . . ?
O10 C5 C6 122.49(19) . . ?
C1 C6 C5 116.1(2) . . ?
C1 C6 C7 122.18(18) . . ?
C5 C6 C7 121.64(18) . . ?
C6 C7 C32 110.90(16) . . ?
C6 C7 C8 113.61(16) . . ?
C32 C7 C8 111.60(16) . . ?
C16 C11 C12 123.9(2) . . ?
C13 C12 C11 116.11(19) . . ?
C13 C12 C27 122.92(18) . . ?
C11 C12 C27 120.94(19) . . ?
C14 C13 O19 120.50(19) . . ?
C14 C13 C12 122.4(2) . . ?
O19 C13 C12 117.04(19) . . ?
C13 C14 C15 119.4(2) . . ?
O20 C15 C14 121.6(2) . . ?
O20 C15 C16 117.44(19) . . ?
C14 C15 C16 120.92(19) . . ?
C11 C16 C15 117.27(19) . . ?
C11 C16 C17 121.98(19) . . ?
C15 C16 C17 120.74(19) . . ?
C16 C17 C2 110.88(15) . . ?
C16 C17 C18 111.73(16) . . ?
C2 C17 C18 113.70(17) . . ?
C22 C21 C26 123.58(19) . . ?
C21 C22 C23 116.84(19) . . ?
C21 C22 C37 123.71(18) . . ?
C23 C22 C37 119.41(18) . . ?
C24 C23 O29 121.61(19) . . ?
C24 C23 C22 121.54(19) . . ?
O29 C23 C22 116.85(19) . . ?
C23 C24 C25 119.72(19) . . ?
O30 C25 C24 115.50(18) . . ?
O30 C25 C26 122.83(18) . . ?
C24 C25 C26 121.7(2) . . ?
C25 C26 C21 116.59(19) . . ?
C25 C26 C27 120.07(19) . . ?
C21 C26 C27 123.31(18) . . ?
C12 C27 C26 110.76(15) . . ?
C12 C27 C28 111.69(16) . . ?
C26 C27 C28 113.58(17) . . ?
C36 C31 C32 123.92(18) . . ?
C31 C32 C33 116.95(18) . . ?
C31 C32 C7 122.00(17) . . ?
C33 C32 C7 121.05(17) . . ?
O39 C33 C34 121.19(18) . . ?
O39 C33 C32 117.57(18) . . ?
C34 C33 C32 121.16(18) . . ?
C35 C34 C33 119.75(18) . . ?
C34 C35 O40 116.70(18) . . ?
C34 C35 C36 121.37(18) . . ?
O40 C35 C36 121.93(18) . . ?
C31 C36 C35 116.84(18) . . ?
C31 C36 C37 120.42(17) . . ?
C35 C36 C37 122.74(18) . . ?
C22 C37 C38 114.54(16) . . ?
C22 C37 C36 109.61(16) . . ?
C38 C37 C36 111.51(16) . . ?
C42 C41 C46 118.1(2) . . ?
C42 C41 C47 122.1(2) . . ?
C46 C41 C47 119.8(2) . . ?
C41 C42 C43 118.6(2) . . ?
N44 C43 C42 123.8(2) . . ?
C43 N44 C45 116.69(19) . . ?
N44 C45 C46 123.8(2) . . ?
C45 C46 C41 119.0(2) . . ?
C48 C47 C41 176.5(2) . . ?
C47 C48 C49 179.5(2) . . ?
C50 C49 C48 179.0(3) . . ?
C49 C50 C51 177.5(2) . . ?
C56 C51 C52 118.20(19) . . ?
C56 C51 C50 120.74(19) . . ?
C52 C51 C50 121.0(2) . . ?
C53 C52 C51 118.5(2) . . ?
N54 C53 C52 123.5(2) . . ?
C55 N54 C53 117.55(19) . . ?
N54 C55 C56 123.4(2) . . ?
C55 C56 C51 118.89(19) . . ?
C62 C61 C66 118.3(2) . . ?
C62 C61 C67 120.5(2) . . ?
C66 C61 C67 121.2(2) . . ?
C63 C62 C61 120.2(2) . . ?
C64 C63 C62 120.3(2) . . ?
C63 C64 C65 120.8(2) . . ?
C64 C65 C66 118.0(2) . . ?
C64 C65 C68 120.5(2) . . ?
C66 C65 C68 121.4(2) . . ?
C65 C66 C61 122.3(2) . . ?
C76 C71 C72 118.9(3) . . ?
C76 C71 C77 123.5(3) . . ?
C72 C71 C77 117.6(3) . . ?
C71 C72 C73 119.9(3) . . ?
C74 C73 C72 120.3(3) . . ?
C75 C74 C73 119.9(3) . . ?
C74 C75 C76 118.9(2) . . ?
C74 C75 C78 121.8(3) . . ?
C76 C75 C78 119.3(3) . . ?
C71 C76 C75 122.1(3) . . ?

_diffrn_measured_fraction_theta_max 0.931
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.931
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.043

#===END

data_nakamura7
_database_code_CSD               214034

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H56 N2 O9'
_chemical_formula_weight         852.99

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                   11.5406(6)
_cell_length_b                   14.0385(8)
_cell_length_c                   15.6820(9)
_cell_angle_alpha                71.7800(10)
_cell_angle_beta                 75.0100(10)
_cell_angle_gamma                65.8730(10)
_cell_volume                     2177.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    116(2)
_cell_measurement_reflns_used    13854
_cell_measurement_theta_min      1.38
_cell_measurement_theta_max      27.92

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             908
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      116(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            13854
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         27.92
_reflns_number_total             9628
_reflns_number_gt                7935
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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^)+(0.0464P)^2^+0.6777P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9628
_refine_ls_number_parameters     610
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1276
_refine_ls_wR_factor_gt          0.1194
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.006
_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 0.36591(15) 0.69128(13) 0.22025(11) 0.0159(3) Uani 1 1 d . . .
H1 H 0.4134 0.6657 0.2676 0.019 Uiso 1 1 calc R . .
C2 C 0.43140(15) 0.69969(13) 0.13189(11) 0.0142(3) Uani 1 1 d . . .
C3 C 0.35833(16) 0.73755(14) 0.06204(11) 0.0185(4) Uani 1 1 d . . .
C4 C 0.22567(16) 0.76655(14) 0.08083(11) 0.0199(4) Uani 1 1 d . . .
H4 H 0.1783 0.7903 0.0336 0.024 Uiso 1 1 calc R . .
C5 C 0.16356(15) 0.76022(13) 0.16957(11) 0.0163(3) Uani 1 1 d . . .
C6 C 0.23368(15) 0.71890(13) 0.24169(11) 0.0148(3) Uani 1 1 d . . .
C7 C 0.16603(15) 0.70209(13) 0.33952(11) 0.0155(3) Uani 1 1 d . . .
H7 H 0.0739 0.7297 0.3366 0.019 Uiso 1 1 calc R . .
C8 C 0.20250(17) 0.58259(14) 0.38487(12) 0.0217(4) Uani 1 1 d . . .
H8A H 0.1878 0.5467 0.3479 0.032 Uiso 1 1 calc R . .
H8B H 0.1510 0.5732 0.4435 0.032 Uiso 1 1 calc R . .
H8C H 0.2916 0.5526 0.3918 0.032 Uiso 1 1 calc R . .
O9 O 0.42123(13) 0.74799(15) -0.02493(9) 0.0422(5) Uani 1 1 d . . .
O10 O 0.03259(11) 0.79698(11) 0.18963(8) 0.0226(3) Uani 1 1 d . . .
C11 C 0.27053(15) 0.72182(13) 0.45503(11) 0.0150(3) Uani 1 1 d . . .
H11 H 0.3180 0.6486 0.4642 0.018 Uiso 1 1 calc R . .
C12 C 0.18520(15) 0.76710(13) 0.39232(11) 0.0147(3) Uani 1 1 d . . .
C13 C 0.11649(15) 0.87718(14) 0.37899(11) 0.0162(3) Uani 1 1 d . . .
C14 C 0.12931(16) 0.93727(14) 0.42881(11) 0.0186(4) Uani 1 1 d . . .
H14 H 0.0802 1.0101 0.4207 0.022 Uiso 1 1 calc R . .
C15 C 0.21485(15) 0.88935(14) 0.49055(11) 0.0167(3) Uani 1 1 d . . .
C16 C 0.28901(15) 0.77981(14) 0.50478(11) 0.0153(3) Uani 1 1 d . . .
C17 C 0.38730(15) 0.72844(14) 0.56963(11) 0.0169(3) Uani 1 1 d . . .
H17 H 0.3470 0.7579 0.6236 0.020 Uiso 1 1 calc R . .
C18 C 0.42451(17) 0.60670(14) 0.60209(12) 0.0211(4) Uani 1 1 d . . .
H18A H 0.4861 0.5791 0.6430 0.032 Uiso 1 1 calc R . .
H18B H 0.4614 0.5748 0.5508 0.032 Uiso 1 1 calc R . .
H18C H 0.3494 0.5897 0.6329 0.032 Uiso 1 1 calc R . .
O19 O 0.03511(12) 0.93255(10) 0.31516(8) 0.0211(3) Uani 1 1 d . . .
O20 O 0.22361(12) 0.95521(10) 0.53588(9) 0.0225(3) Uani 1 1 d . . .
C21 C 0.59525(15) 0.71892(13) 0.45904(11) 0.0160(3) Uani 1 1 d . . .
H21 H 0.5830 0.6695 0.4376 0.019 Uiso 1 1 calc R . .
C22 C 0.50507(15) 0.76064(14) 0.52878(11) 0.0160(3) Uani 1 1 d . . .
C23 C 0.52393(15) 0.83638(14) 0.55835(11) 0.0170(3) Uani 1 1 d . . .
C24 C 0.63034(16) 0.86702(14) 0.52075(11) 0.0180(3) Uani 1 1 d . . .
H24 H 0.6422 0.9172 0.5415 0.022 Uiso 1 1 calc R . .
C25 C 0.71810(15) 0.82236(14) 0.45244(11) 0.0168(3) Uani 1 1 d . . .
C26 C 0.70288(15) 0.74730(13) 0.41971(11) 0.0154(3) Uani 1 1 d . . .
C27 C 0.79584(15) 0.70315(13) 0.34054(11) 0.0152(3) Uani 1 1 d . . .
H27 H 0.8660 0.7304 0.3269 0.018 Uiso 1 1 calc R . .
C28 C 0.85605(16) 0.58075(14) 0.36485(12) 0.0202(4) Uani 1 1 d . . .
H28A H 0.8962 0.5576 0.4180 0.030 Uiso 1 1 calc R . .
H28B H 0.9193 0.5569 0.3151 0.030 Uiso 1 1 calc R . .
H28C H 0.7905 0.5508 0.3767 0.030 Uiso 1 1 calc R . .
O29 O 0.43190(11) 0.88330(10) 0.62302(8) 0.0201(3) Uani 1 1 d . . .
O30 O 0.82239(11) 0.85326(11) 0.41087(8) 0.0205(3) Uani 1 1 d . . .
C31 C 0.68847(15) 0.68974(13) 0.22252(11) 0.0146(3) Uani 1 1 d . . .
H31 H 0.7074 0.6172 0.2502 0.017 Uiso 1 1 calc R . .
C32 C 0.72951(14) 0.74896(13) 0.25658(11) 0.0140(3) Uani 1 1 d . . .
C33 C 0.70211(15) 0.85734(13) 0.21247(11) 0.0156(3) Uani 1 1 d . . .
C34 C 0.63372(15) 0.90376(13) 0.14049(11) 0.0160(3) Uani 1 1 d . . .
H34 H 0.6155 0.9762 0.1126 0.019 Uiso 1 1 calc R . .
C35 C 0.59244(15) 0.84265(13) 0.10996(11) 0.0148(3) Uani 1 1 d . . .
C36 C 0.62070(15) 0.73291(13) 0.14940(11) 0.0142(3) Uani 1 1 d . . .
C37 C 0.57675(15) 0.66882(13) 0.11091(11) 0.0148(3) Uani 1 1 d . . .
H37 H 0.5984 0.6892 0.0447 0.018 Uiso 1 1 calc R . .
C38 C 0.64408(16) 0.54752(14) 0.13957(12) 0.0207(4) Uani 1 1 d . . .
H38A H 0.6117 0.5125 0.1126 0.031 Uiso 1 1 calc R . .
H38B H 0.6280 0.5244 0.2045 0.031 Uiso 1 1 calc R . .
H38C H 0.7348 0.5293 0.1197 0.031 Uiso 1 1 calc R . .
O39 O 0.74074(12) 0.92380(10) 0.23797(9) 0.0199(3) Uani 1 1 d . . .
O40 O 0.52294(12) 0.89095(11) 0.03908(8) 0.0186(3) Uani 1 1 d . . .
C41 C 0.78825(16) 0.89218(15) -0.09879(11) 0.0200(4) Uani 1 1 d . . .
C42 C 0.85299(18) 0.78922(16) -0.05057(13) 0.0273(4) Uani 1 1 d . . .
H42 H 0.8504 0.7293 -0.0624 0.033 Uiso 1 1 calc R . .
C43 C 0.92102(18) 0.77750(17) 0.01496(13) 0.0298(4) Uani 1 1 d . . .
H43 H 0.9626 0.7084 0.0472 0.036 Uiso 1 1 calc R . .
N44 N 0.93046(14) 0.85943(14) 0.03468(10) 0.0258(4) Uani 1 1 d . . .
C45 C 0.87095(16) 0.95781(17) -0.01323(12) 0.0245(4) Uani 1 1 d . . .
H45 H 0.8777 1.0160 -0.0013 0.029 Uiso 1 1 calc R . .
C46 C 0.79980(16) 0.97750(15) -0.07968(12) 0.0212(4) Uani 1 1 d . . .
H46 H 0.7601 1.0474 -0.1113 0.025 Uiso 1 1 calc R . .
C47 C 0.70700(15) 0.90880(14) -0.16568(11) 0.0179(3) Uani 1 1 d . . .
C48 C 0.67850(16) 1.00019(15) -0.23613(11) 0.0210(4) Uani 1 1 d . . .
H48 H 0.7114 1.0531 -0.2434 0.025 Uiso 1 1 calc R . .
C49 C 0.60067(16) 1.01178(16) -0.29545(12) 0.0222(4) Uani 1 1 d . . .
H49 H 0.5829 1.0732 -0.3425 0.027 Uiso 1 1 calc R . .
N50 N 0.55008(13) 0.93921(12) -0.28843(10) 0.0198(3) Uani 1 1 d . . .
C51 C 0.57628(17) 0.85233(15) -0.21995(12) 0.0226(4) Uani 1 1 d . . .
H51 H 0.5407 0.8014 -0.2137 0.027 Uiso 1 1 calc R . .
C52 C 0.65305(18) 0.83396(15) -0.15808(12) 0.0234(4) Uani 1 1 d . . .
H52 H 0.6686 0.7719 -0.1116 0.028 Uiso 1 1 calc R . .
C61 C 0.2350(2) 0.43034(16) 0.19194(16) 0.0349(5) Uani 1 1 d . . .
C62 C 0.1580(2) 0.47669(18) 0.12402(17) 0.0435(6) Uani 1 1 d . . .
H62 H 0.1830 0.5196 0.0698 0.052 Uiso 1 1 calc R . .
C63 C 0.0451(2) 0.4596(2) 0.13626(17) 0.0451(6) Uani 1 1 d . . .
H63 H -0.0062 0.4918 0.0907 0.054 Uiso 1 1 calc R . .
C64 C 0.0077(2) 0.39509(18) 0.21570(17) 0.0401(5) Uani 1 1 d . . .
H64 H -0.0684 0.3833 0.2231 0.048 Uiso 1 1 calc R . .
C65 C 0.08228(19) 0.34760(17) 0.28469(16) 0.0348(5) Uani 1 1 d . . .
C66 C 0.19447(19) 0.36745(16) 0.27153(16) 0.0333(5) Uani 1 1 d . . .
H66 H 0.2442 0.3373 0.3180 0.040 Uiso 1 1 calc R . .
C67 C 0.3599(2) 0.4469(2) 0.1773(2) 0.0527(7) Uani 1 1 d . . .
H67A H 0.4005 0.4097 0.2306 0.079 Uiso 1 1 calc R . .
H67B H 0.3439 0.5222 0.1655 0.079 Uiso 1 1 calc R . .
H67C H 0.4151 0.4194 0.1264 0.079 Uiso 1 1 calc R . .
C68 C 0.0445(3) 0.2756(2) 0.3723(2) 0.0609(8) Uani 1 1 d . . .
H68A H -0.0415 0.2800 0.3749 0.091 Uiso 1 1 calc R . .
H68B H 0.0487 0.2983 0.4228 0.091 Uiso 1 1 calc R . .
H68C H 0.1023 0.2028 0.3747 0.091 Uiso 1 1 calc R . .
O71 O 0.74416(15) 0.12380(12) 0.14286(10) 0.0331(4) Uani 1 1 d . . .
C72 C 0.81871(18) 0.14529(16) 0.18825(13) 0.0263(4) Uani 1 1 d . . .
H72A H 0.9092 0.1150 0.1650 0.032 Uiso 1 1 calc R . .
H72B H 0.8056 0.1133 0.2528 0.032 Uiso 1 1 calc R . .
C73 C 0.7779(3) 0.2642(2) 0.17249(19) 0.0547(7) Uani 1 1 d . . .
H73A H 0.8273 0.2805 0.2029 0.082 Uiso 1 1 calc R . .
H73B H 0.6884 0.2933 0.1959 0.082 Uiso 1 1 calc R . .
H73C H 0.7916 0.2951 0.1085 0.082 Uiso 1 1 calc R . .
H9 H 0.368(2) 0.781(2) -0.0602(17) 0.047(7) Uiso 1 1 d . . .
H10 H -0.004(2) 0.8225(19) 0.1373(16) 0.043(7) Uiso 1 1 d . . .
H19 H 0.034(2) 0.891(2) 0.2873(17) 0.043(7) Uiso 1 1 d . . .
H20 H 0.285(2) 0.9213(18) 0.5686(15) 0.037(6) Uiso 1 1 d . . .
H29 H 0.466(2) 0.918(2) 0.6470(17) 0.052(7) Uiso 1 1 d . . .
H30 H 0.818(2) 0.906(2) 0.4340(16) 0.047(7) Uiso 1 1 d . . .
H39 H 0.780(2) 0.893(2) 0.2849(17) 0.045(7) Uiso 1 1 d . . .
H40A H 0.506(4) 0.851(3) 0.021(3) 0.041(12) Uiso 0.60 1 d P . .
H40B H 0.512(4) 0.960(4) 0.027(3) 0.013(12) Uiso 0.40 1 d P . .
H71 H 0.740(2) 0.061(2) 0.1684(18) 0.053(8) Uiso 1 1 d . . .

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 0.0159(8) 0.0174(8) 0.0149(8) -0.0006(6) -0.0080(6) -0.0053(7)
C2 0.0141(8) 0.0113(7) 0.0179(8) -0.0014(6) -0.0048(6) -0.0054(6)
C3 0.0176(8) 0.0231(9) 0.0141(8) -0.0024(7) -0.0032(6) -0.0076(7)
C4 0.0164(8) 0.0265(9) 0.0161(8) -0.0026(7) -0.0077(6) -0.0055(7)
C5 0.0143(8) 0.0177(8) 0.0184(8) -0.0028(7) -0.0037(6) -0.0074(7)
C6 0.0156(8) 0.0156(8) 0.0143(8) -0.0027(6) -0.0027(6) -0.0071(7)
C7 0.0124(7) 0.0208(8) 0.0136(8) -0.0024(6) -0.0035(6) -0.0065(7)
C8 0.0277(9) 0.0236(9) 0.0177(9) -0.0016(7) -0.0050(7) -0.0145(8)
O9 0.0156(7) 0.0865(13) 0.0122(7) -0.0043(7) -0.0038(5) -0.0105(8)
O10 0.0118(6) 0.0357(7) 0.0174(6) -0.0039(5) -0.0058(5) -0.0052(5)
C11 0.0116(7) 0.0160(8) 0.0149(8) -0.0017(6) -0.0012(6) -0.0044(6)
C12 0.0124(7) 0.0193(8) 0.0133(8) -0.0035(6) -0.0001(6) -0.0079(7)
C13 0.0110(7) 0.0216(9) 0.0144(8) -0.0006(6) -0.0027(6) -0.0064(7)
C14 0.0144(8) 0.0156(8) 0.0217(9) -0.0025(7) -0.0004(6) -0.0040(7)
C15 0.0149(8) 0.0220(9) 0.0160(8) -0.0070(7) 0.0013(6) -0.0096(7)
C16 0.0114(7) 0.0216(9) 0.0126(8) -0.0027(6) -0.0001(6) -0.0075(7)
C17 0.0158(8) 0.0224(9) 0.0141(8) -0.0040(7) -0.0024(6) -0.0085(7)
C18 0.0211(9) 0.0236(9) 0.0196(9) 0.0033(7) -0.0094(7) -0.0112(8)
O19 0.0189(6) 0.0207(7) 0.0213(7) -0.0008(5) -0.0097(5) -0.0038(5)
O20 0.0197(6) 0.0231(7) 0.0287(7) -0.0115(6) -0.0060(5) -0.0061(6)
C21 0.0177(8) 0.0165(8) 0.0165(8) -0.0033(6) -0.0069(6) -0.0066(7)
C22 0.0139(8) 0.0203(8) 0.0142(8) -0.0009(6) -0.0054(6) -0.0070(7)
C23 0.0144(8) 0.0222(9) 0.0144(8) -0.0041(7) -0.0033(6) -0.0060(7)
C24 0.0184(8) 0.0219(9) 0.0182(8) -0.0068(7) -0.0046(6) -0.0087(7)
C25 0.0144(8) 0.0211(9) 0.0167(8) -0.0025(7) -0.0045(6) -0.0081(7)
C26 0.0137(8) 0.0166(8) 0.0149(8) -0.0037(6) -0.0037(6) -0.0038(7)
C27 0.0124(7) 0.0167(8) 0.0173(8) -0.0055(6) -0.0028(6) -0.0047(6)
C28 0.0194(8) 0.0189(9) 0.0204(9) -0.0045(7) -0.0074(7) -0.0022(7)
O29 0.0154(6) 0.0312(7) 0.0192(6) -0.0128(5) -0.0004(5) -0.0101(5)
O30 0.0174(6) 0.0269(7) 0.0230(6) -0.0115(5) 0.0016(5) -0.0123(5)
C31 0.0134(7) 0.0125(8) 0.0160(8) -0.0017(6) -0.0012(6) -0.0047(6)
C32 0.0096(7) 0.0142(8) 0.0164(8) -0.0033(6) -0.0012(6) -0.0033(6)
C33 0.0121(7) 0.0156(8) 0.0196(8) -0.0052(7) 0.0001(6) -0.0061(6)
C34 0.0137(8) 0.0106(7) 0.0191(8) -0.0003(6) -0.0009(6) -0.0031(6)
C35 0.0098(7) 0.0170(8) 0.0145(8) -0.0011(6) -0.0022(6) -0.0035(6)
C36 0.0098(7) 0.0148(8) 0.0170(8) -0.0033(6) -0.0010(6) -0.0043(6)
C37 0.0142(8) 0.0167(8) 0.0134(8) -0.0030(6) -0.0037(6) -0.0049(7)
C38 0.0191(8) 0.0171(8) 0.0276(9) -0.0085(7) -0.0071(7) -0.0036(7)
O39 0.0207(6) 0.0167(6) 0.0257(7) -0.0043(5) -0.0070(5) -0.0082(5)
O40 0.0200(6) 0.0155(6) 0.0219(6) -0.0012(5) -0.0102(5) -0.0060(5)
C41 0.0125(8) 0.0290(10) 0.0163(8) -0.0070(7) -0.0017(6) -0.0043(7)
C42 0.0238(9) 0.0260(10) 0.0269(10) -0.0104(8) -0.0077(8) 0.0017(8)
C43 0.0214(9) 0.0328(11) 0.0253(10) -0.0072(8) -0.0098(8) 0.0043(8)
N44 0.0140(7) 0.0416(10) 0.0193(8) -0.0086(7) -0.0043(6) -0.0052(7)
C45 0.0174(8) 0.0372(11) 0.0209(9) -0.0069(8) -0.0031(7) -0.0114(8)
C46 0.0160(8) 0.0306(10) 0.0169(8) -0.0039(7) -0.0028(6) -0.0092(8)
C47 0.0128(8) 0.0246(9) 0.0150(8) -0.0087(7) -0.0008(6) -0.0032(7)
C48 0.0192(8) 0.0293(10) 0.0168(8) -0.0038(7) -0.0013(7) -0.0129(8)
C49 0.0184(8) 0.0312(10) 0.0150(8) -0.0023(7) -0.0029(7) -0.0092(8)
N50 0.0149(7) 0.0283(8) 0.0165(7) -0.0103(6) -0.0008(5) -0.0054(6)
C51 0.0237(9) 0.0244(9) 0.0236(9) -0.0111(7) -0.0051(7) -0.0077(8)
C52 0.0291(10) 0.0200(9) 0.0211(9) -0.0050(7) -0.0086(7) -0.0059(8)
C61 0.0297(11) 0.0240(10) 0.0542(14) -0.0204(10) -0.0035(10) -0.0061(9)
C62 0.0499(14) 0.0313(12) 0.0427(13) -0.0081(10) -0.0037(11) -0.0106(11)
C63 0.0466(14) 0.0411(14) 0.0494(15) -0.0170(11) -0.0172(12) -0.0070(11)
C64 0.0283(11) 0.0382(13) 0.0614(16) -0.0264(12) -0.0088(10) -0.0075(10)
C65 0.0268(10) 0.0254(10) 0.0490(13) -0.0177(10) 0.0011(9) -0.0035(9)
C66 0.0270(10) 0.0268(11) 0.0462(13) -0.0172(9) -0.0087(9) -0.0015(9)
C67 0.0399(13) 0.0373(14) 0.086(2) -0.0271(14) 0.0031(13) -0.0170(11)
C68 0.0487(15) 0.0508(17) 0.0669(19) -0.0067(14) 0.0077(13) -0.0168(13)
O71 0.0477(9) 0.0299(8) 0.0307(8) 0.0078(6) -0.0247(7) -0.0225(7)
C72 0.0258(9) 0.0312(10) 0.0262(10) -0.0066(8) -0.0055(8) -0.0136(8)
C73 0.081(2) 0.0383(14) 0.0553(16) -0.0173(12) -0.0021(14) -0.0316(14)

_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 1.387(2) . ?
C1 C2 1.391(2) . ?
C2 C3 1.393(2) . ?
C2 C37 1.523(2) . ?
C3 O9 1.363(2) . ?
C3 C4 1.389(2) . ?
C4 C5 1.385(2) . ?
C5 O10 1.3666(19) . ?
C5 C6 1.396(2) . ?
C6 C7 1.524(2) . ?
C7 C12 1.517(2) . ?
C7 C8 1.526(2) . ?
C11 C12 1.393(2) . ?
C11 C16 1.394(2) . ?
C12 C13 1.394(2) . ?
C13 O19 1.3752(19) . ?
C13 C14 1.385(2) . ?
C14 C15 1.382(2) . ?
C15 O20 1.377(2) . ?
C15 C16 1.398(2) . ?
C16 C17 1.520(2) . ?
C17 C22 1.527(2) . ?
C17 C18 1.528(2) . ?
C21 C22 1.391(2) . ?
C21 C26 1.392(2) . ?
C22 C23 1.394(2) . ?
C23 O29 1.371(2) . ?
C23 C24 1.393(2) . ?
C24 C25 1.381(2) . ?
C25 O30 1.3805(19) . ?
C25 C26 1.393(2) . ?
C26 C27 1.525(2) . ?
C27 C32 1.524(2) . ?
C27 C28 1.527(2) . ?
C31 C32 1.390(2) . ?
C31 C36 1.391(2) . ?
C32 C33 1.398(2) . ?
C33 O39 1.377(2) . ?
C33 C34 1.379(2) . ?
C34 C35 1.379(2) . ?
C35 O40 1.3725(19) . ?
C35 C36 1.400(2) . ?
C36 C37 1.517(2) . ?
C37 C38 1.525(2) . ?
C41 C46 1.385(3) . ?
C41 C42 1.395(2) . ?
C41 C47 1.487(2) . ?
C42 C43 1.380(3) . ?
C43 N44 1.331(3) . ?
N44 C45 1.336(2) . ?
C45 C46 1.383(2) . ?
C47 C52 1.387(3) . ?
C47 C48 1.390(2) . ?
C48 C49 1.385(2) . ?
C49 N50 1.332(2) . ?
N50 C51 1.334(2) . ?
C51 C52 1.376(2) . ?
C61 C66 1.379(3) . ?
C61 C62 1.390(3) . ?
C61 C67 1.501(3) . ?
C62 C63 1.373(3) . ?
C63 C64 1.377(3) . ?
C64 C65 1.385(3) . ?
C65 C66 1.385(3) . ?
C65 C68 1.510(3) . ?
O71 C72 1.415(2) . ?
C72 C73 1.492(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
C6 C1 C2 123.69(15) . . ?
C1 C2 C3 117.15(14) . . ?
C1 C2 C37 122.23(14) . . ?
C3 C2 C37 120.61(14) . . ?
O9 C3 C4 121.50(15) . . ?
O9 C3 C2 117.67(15) . . ?
C4 C3 C2 120.80(15) . . ?
C5 C4 C3 120.33(15) . . ?
O10 C5 C4 121.64(15) . . ?
O10 C5 C6 117.74(15) . . ?
C4 C5 C6 120.59(15) . . ?
C1 C6 C5 117.33(15) . . ?
C1 C6 C7 122.21(14) . . ?
C5 C6 C7 120.44(14) . . ?
C12 C7 C6 112.03(13) . . ?
C12 C7 C8 114.08(13) . . ?
C6 C7 C8 110.62(14) . . ?
C12 C11 C16 123.82(16) . . ?
C11 C12 C13 116.93(15) . . ?
C11 C12 C7 122.83(15) . . ?
C13 C12 C7 120.23(14) . . ?
O19 C13 C14 116.32(15) . . ?
O19 C13 C12 122.57(15) . . ?
C14 C13 C12 121.10(15) . . ?
C15 C14 C13 120.19(16) . . ?
O20 C15 C14 116.50(16) . . ?
O20 C15 C16 122.38(15) . . ?
C14 C15 C16 121.12(16) . . ?
C11 C16 C15 116.78(15) . . ?
C11 C16 C17 122.26(15) . . ?
C15 C16 C17 120.94(15) . . ?
C16 C17 C22 110.96(13) . . ?
C16 C17 C18 113.41(14) . . ?
C22 C17 C18 111.71(14) . . ?
C22 C21 C26 123.39(16) . . ?
C21 C22 C23 117.26(15) . . ?
C21 C22 C17 121.91(15) . . ?
C23 C22 C17 120.79(15) . . ?
O29 C23 C24 120.74(15) . . ?
O29 C23 C22 118.07(14) . . ?
C24 C23 C22 121.14(16) . . ?
C25 C24 C23 119.47(16) . . ?
O30 C25 C24 121.46(15) . . ?
O30 C25 C26 116.85(15) . . ?
C24 C25 C26 121.64(15) . . ?
C21 C26 C25 117.08(15) . . ?
C21 C26 C27 121.42(15) . . ?
C25 C26 C27 121.40(14) . . ?
C32 C27 C26 109.53(13) . . ?
C32 C27 C28 114.01(14) . . ?
C26 C27 C28 112.29(14) . . ?
C32 C31 C36 123.70(15) . . ?
C31 C32 C33 116.88(15) . . ?
C31 C32 C27 123.49(14) . . ?
C33 C32 C27 119.57(15) . . ?
O39 C33 C34 116.16(14) . . ?
O39 C33 C32 122.52(15) . . ?
C34 C33 C32 121.33(15) . . ?
C35 C34 C33 119.94(15) . . ?
O40 C35 C34 118.90(15) . . ?
O40 C35 C36 119.77(15) . . ?
C34 C35 C36 121.33(15) . . ?
C31 C36 C35 116.76(15) . . ?
C31 C36 C37 124.19(15) . . ?
C35 C36 C37 119.05(14) . . ?
C36 C37 C2 111.15(13) . . ?
C36 C37 C38 114.21(13) . . ?
C2 C37 C38 110.98(13) . . ?
C46 C41 C42 117.31(16) . . ?
C46 C41 C47 121.83(16) . . ?
C42 C41 C47 120.83(17) . . ?
C43 C42 C41 119.10(19) . . ?
N44 C43 C42 123.76(18) . . ?
C43 N44 C45 116.97(16) . . ?
N44 C45 C46 123.39(19) . . ?
C45 C46 C41 119.44(17) . . ?
C52 C47 C48 117.22(16) . . ?
C52 C47 C41 120.61(16) . . ?
C48 C47 C41 122.14(16) . . ?
C49 C48 C47 119.43(17) . . ?
N50 C49 C48 123.15(17) . . ?
C49 N50 C51 117.19(15) . . ?
N50 C51 C52 123.60(17) . . ?
C51 C52 C47 119.41(17) . . ?
C66 C61 C62 118.0(2) . . ?
C66 C61 C67 121.6(2) . . ?
C62 C61 C67 120.4(2) . . ?
C63 C62 C61 120.6(2) . . ?
C62 C63 C64 120.3(2) . . ?
C63 C64 C65 120.5(2) . . ?
C66 C65 C64 118.1(2) . . ?
C66 C65 C68 120.0(2) . . ?
C64 C65 C68 121.8(2) . . ?
C61 C66 C65 122.3(2) . . ?
O71 C72 C73 108.13(17) . . ?

_diffrn_measured_fraction_theta_max 0.923
_diffrn_reflns_theta_full        27.92
_diffrn_measured_fraction_theta_full 0.923
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.048

#===END

data_nakamura8
_database_code_CSD               214035

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C63 H66 N4 O9'
_chemical_formula_weight         1023.20

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)/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                   20.7807(17)
_cell_length_b                   16.3390(14)
_cell_length_c                   15.4817(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.073(2)
_cell_angle_gamma                90.00
_cell_volume                     5204.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    116(2)
_cell_measurement_reflns_used    30419
_cell_measurement_theta_min      1.59
_cell_measurement_theta_max      27.90

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2176
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      116(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            30419
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         27.90
_reflns_number_total             11763
_reflns_number_gt                7620
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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^)+(0.0834P)^2^+2.2894P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11763
_refine_ls_number_parameters     730
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1701
_refine_ls_wR_factor_gt          0.1460
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.011
_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 0.93560(9) -0.00676(11) 0.28274(13) 0.0203(4) Uani 1 1 d . . .
H1 H 0.9132 -0.0064 0.3307 0.024 Uiso 1 1 calc R . .
C2 C 0.95229(8) 0.06808(12) 0.24878(13) 0.0203(4) Uani 1 1 d . . .
C3 C 0.98374(9) 0.06583(12) 0.17539(14) 0.0230(4) Uani 1 1 d . . .
C4 C 0.99815(9) -0.00771(12) 0.13806(14) 0.0232(4) Uani 1 1 d . . .
H4 H 1.0184 -0.0081 0.0882 0.028 Uiso 1 1 calc R . .
C5 C 0.98231(9) -0.08071(12) 0.17533(14) 0.0226(4) Uani 1 1 d . . .
C6 C 0.95075(9) -0.08214(12) 0.24866(13) 0.0206(4) Uani 1 1 d . . .
C7 C 0.93305(9) -0.16267(11) 0.28855(13) 0.0206(4) Uani 1 1 d . . .
H7 H 0.9620 -0.2044 0.2697 0.025 Uiso 1 1 calc R . .
C8 C 0.94520(9) -0.16164(12) 0.38812(13) 0.0237(4) Uani 1 1 d . . .
H8A H 0.9337 -0.2138 0.4101 0.036 Uiso 1 1 calc R . .
H8B H 0.9192 -0.1196 0.4094 0.036 Uiso 1 1 calc R . .
H8C H 0.9903 -0.1509 0.4075 0.036 Uiso 1 1 calc R . .
O9 O 0.99935(7) 0.13887(9) 0.13862(10) 0.0271(3) Uani 1 1 d . . .
O10 O 0.99659(7) -0.15404(9) 0.13823(10) 0.0262(3) Uani 1 1 d . . .
C11 C 0.81092(9) -0.16175(11) 0.29065(13) 0.0194(4) Uani 1 1 d . . .
H11 H 0.8189 -0.1290 0.3401 0.023 Uiso 1 1 calc R . .
C12 C 0.86378(9) -0.18813(11) 0.25228(13) 0.0197(4) Uani 1 1 d . . .
C13 C 0.85077(9) -0.23687(12) 0.17815(13) 0.0215(4) Uani 1 1 d . . .
C14 C 0.78759(9) -0.25722(12) 0.14449(13) 0.0220(4) Uani 1 1 d . . .
H14 H 0.7797 -0.2907 0.0956 0.026 Uiso 1 1 calc R . .
C15 C 0.73592(9) -0.22799(11) 0.18324(13) 0.0196(4) Uani 1 1 d . . .
C16 C 0.74659(9) -0.18137(11) 0.25949(12) 0.0184(4) Uani 1 1 d . . .
C17 C 0.69059(9) -0.15372(11) 0.30631(12) 0.0189(4) Uani 1 1 d . . .
H17 H 0.6559 -0.1941 0.2920 0.023 Uiso 1 1 calc R . .
C18 C 0.70800(9) -0.15492(12) 0.40546(13) 0.0235(4) Uani 1 1 d . . .
H18A H 0.7251 -0.2077 0.4237 0.035 Uiso 1 1 calc R . .
H18B H 0.6698 -0.1441 0.4319 0.035 Uiso 1 1 calc R . .
H18C H 0.7401 -0.1137 0.4230 0.035 Uiso 1 1 calc R . .
O19 O 0.89877(7) -0.26951(9) 0.13582(10) 0.0289(4) Uani 1 1 d . . .
O20 O 0.67521(6) -0.25060(9) 0.14423(9) 0.0238(3) Uani 1 1 d . . .
C21 C 0.68959(9) 0.00205(11) 0.30349(13) 0.0186(4) Uani 1 1 d . . .
H21 H 0.7265 0.0006 0.3452 0.022 Uiso 1 1 calc R . .
C22 C 0.66274(8) -0.07196(11) 0.27220(12) 0.0183(4) Uani 1 1 d . . .
C23 C 0.60852(9) -0.06835(11) 0.20848(13) 0.0194(4) Uani 1 1 d . . .
C24 C 0.58284(9) 0.00610(11) 0.17793(13) 0.0203(4) Uani 1 1 d . . .
H24 H 0.5471 0.0075 0.1344 0.024 Uiso 1 1 calc R . .
C25 C 0.61031(9) 0.07848(11) 0.21207(12) 0.0184(4) Uani 1 1 d . . .
C26 C 0.66451(8) 0.07791(11) 0.27609(12) 0.0184(4) Uani 1 1 d . . .
C27 C 0.69583(9) 0.15737(11) 0.31222(12) 0.0189(4) Uani 1 1 d . . .
H27 H 0.6628 0.2003 0.3005 0.023 Uiso 1 1 calc R . .
C28 C 0.71548(9) 0.15448(12) 0.41114(13) 0.0234(4) Uani 1 1 d . . .
H28A H 0.7347 0.2058 0.4309 0.035 Uiso 1 1 calc R . .
H28B H 0.7463 0.1112 0.4257 0.035 Uiso 1 1 calc R . .
H28C H 0.6777 0.1447 0.4389 0.035 Uiso 1 1 calc R . .
O29 O 0.58102(6) -0.14052(8) 0.17597(9) 0.0234(3) Uani 1 1 d . . .
O30 O 0.58434(6) 0.15248(8) 0.18299(9) 0.0228(3) Uani 1 1 d . . .
C31 C 0.81493(9) 0.15588(11) 0.29203(13) 0.0193(4) Uani 1 1 d . . .
H31 H 0.8220 0.1218 0.3405 0.023 Uiso 1 1 calc R . .
C32 C 0.75172(9) 0.18115(11) 0.26383(12) 0.0187(4) Uani 1 1 d . . .
C33 C 0.74220(9) 0.22985(11) 0.18900(13) 0.0189(4) Uani 1 1 d . . .
C34 C 0.79378(9) 0.25344(12) 0.14786(13) 0.0213(4) Uani 1 1 d . . .
H34 H 0.7866 0.2868 0.0988 0.026 Uiso 1 1 calc R . .
C35 C 0.85650(9) 0.22787(12) 0.17907(13) 0.0220(4) Uani 1 1 d . . .
C36 C 0.86818(9) 0.17818(11) 0.25267(13) 0.0197(4) Uani 1 1 d . . .
C37 C 0.93657(9) 0.14963(11) 0.28881(13) 0.0208(4) Uani 1 1 d . . .
H37 H 0.9666 0.1900 0.2699 0.025 Uiso 1 1 calc R . .
C38 C 0.94885(9) 0.14867(12) 0.38840(13) 0.0250(4) Uani 1 1 d . . .
H38A H 0.9385 0.2013 0.4103 0.038 Uiso 1 1 calc R . .
H38B H 0.9938 0.1365 0.4077 0.038 Uiso 1 1 calc R . .
H38C H 0.9220 0.1077 0.4098 0.038 Uiso 1 1 calc R . .
O39 O 0.68220(7) 0.25963(9) 0.15421(9) 0.0246(3) Uani 1 1 d . . .
O40 O 0.90470(7) 0.25679(9) 0.13507(10) 0.0279(3) Uani 1 1 d . . .
C41 C 0.75229(9) 0.11319(11) -0.09299(13) 0.0209(4) Uani 1 1 d . . .
C42 C 0.79341(9) 0.10968(13) -0.01434(14) 0.0270(5) Uani 1 1 d . . .
H42 H 0.7766 0.1031 0.0378 0.032 Uiso 1 1 calc R . .
C43 C 0.85975(10) 0.11605(14) -0.01440(15) 0.0309(5) Uani 1 1 d . . .
H43 H 0.8868 0.1133 0.0387 0.037 Uiso 1 1 calc R . .
N44 N 0.88689(8) 0.12597(11) -0.08677(12) 0.0288(4) Uani 1 1 d . . .
C45 C 0.84739(10) 0.12736(12) -0.16216(15) 0.0272(5) Uani 1 1 d . . .
H45 H 0.8657 0.1329 -0.2134 0.033 Uiso 1 1 calc R . .
C46 C 0.78062(9) 0.12100(12) -0.16835(14) 0.0238(4) Uani 1 1 d . . .
H46 H 0.7549 0.1220 -0.2226 0.029 Uiso 1 1 calc R . .
C47 C 0.68068(9) 0.11169(11) -0.09700(13) 0.0201(4) Uani 1 1 d . . .
C48 C 0.64115(9) 0.07769(12) -0.16761(13) 0.0241(4) Uani 1 1 d . . .
H48 H 0.6594 0.0536 -0.2129 0.029 Uiso 1 1 calc R . .
C49 C 0.57476(10) 0.07986(13) -0.17007(14) 0.0256(5) Uani 1 1 d . . .
H49 H 0.5492 0.0555 -0.2172 0.031 Uiso 1 1 calc R . .
N50 N 0.54508(8) 0.11487(10) -0.10875(11) 0.0249(4) Uani 1 1 d . . .
C51 C 0.58326(9) 0.14753(12) -0.04050(14) 0.0245(4) Uani 1 1 d . . .
H51 H 0.5636 0.1720 0.0033 0.029 Uiso 1 1 calc R . .
C52 C 0.65017(9) 0.14663(12) -0.03198(13) 0.0234(4) Uani 1 1 d . . .
H52 H 0.6747 0.1693 0.0171 0.028 Uiso 1 1 calc R . .
C61 C 0.74931(9) -0.11236(11) -0.09572(13) 0.0221(4) Uani 1 1 d . . .
C62 C 0.77899(10) -0.10818(13) -0.17033(15) 0.0281(5) Uani 1 1 d . . .
H62 H 0.7541 -0.1040 -0.2250 0.034 Uiso 1 1 calc R . .
C63 C 0.84609(10) -0.11032(13) -0.16258(16) 0.0309(5) Uani 1 1 d . . .
H63 H 0.8654 -0.1082 -0.2132 0.037 Uiso 1 1 calc R . .
N64 N 0.88444(8) -0.11530(11) -0.08647(13) 0.0321(4) Uani 1 1 d . . .
C65 C 0.85595(10) -0.11694(15) -0.01481(16) 0.0360(6) Uani 1 1 d . . .
H65 H 0.8821 -0.1190 0.0390 0.043 Uiso 1 1 calc R . .
C66 C 0.78915(9) -0.11567(14) -0.01641(15) 0.0301(5) Uani 1 1 d . . .
H66 H 0.7713 -0.1170 0.0354 0.036 Uiso 1 1 calc R . .
C67 C 0.67730(9) -0.11693(11) -0.10142(13) 0.0205(4) Uani 1 1 d . . .
C68 C 0.63997(9) -0.14326(12) -0.17783(14) 0.0236(4) Uani 1 1 d . . .
H68 H 0.6596 -0.1563 -0.2264 0.028 Uiso 1 1 calc R . .
C69 C 0.57379(9) -0.14994(12) -0.18116(14) 0.0257(5) Uani 1 1 d . . .
H69 H 0.5499 -0.1685 -0.2327 0.031 Uiso 1 1 calc R . .
N70 N 0.54181(8) -0.13146(10) -0.11506(11) 0.0240(4) Uani 1 1 d . . .
C71 C 0.57745(10) -0.10458(13) -0.04240(14) 0.0281(5) Uani 1 1 d . . .
H71 H 0.5562 -0.0902 0.0044 0.034 Uiso 1 1 calc R . .
C72 C 0.64429(10) -0.09682(13) -0.03253(14) 0.0261(5) Uani 1 1 d . . .
H72 H 0.6669 -0.0783 0.0199 0.031 Uiso 1 1 calc R . .
C81 C 0.61824(10) -0.00641(12) -0.39970(13) 0.0232(4) Uani 1 1 d . . .
C82 C 0.58225(10) -0.07812(12) -0.40007(13) 0.0241(4) Uani 1 1 d . . .
H82 H 0.6028 -0.1282 -0.4041 0.029 Uiso 1 1 calc R . .
C83 C 0.51592(10) -0.07641(12) -0.39452(13) 0.0230(4) Uani 1 1 d . . .
C84 C 0.48600(10) -0.00125(12) -0.38819(13) 0.0223(4) Uani 1 1 d . . .
H84 H 0.4418 0.0005 -0.3839 0.027 Uiso 1 1 calc R . .
C85 C 0.52064(9) 0.07136(12) -0.38807(13) 0.0222(4) Uani 1 1 d . . .
C86 C 0.58677(9) 0.06773(12) -0.39332(13) 0.0231(4) Uani 1 1 d . . .
H86 H 0.6105 0.1161 -0.3925 0.028 Uiso 1 1 calc R . .
C87 C 0.69011(10) -0.00893(14) -0.40546(16) 0.0333(5) Uani 1 1 d . . .
H87A H 0.6968 -0.0037 -0.4653 0.050 Uiso 1 1 calc R . .
H87B H 0.7078 -0.0600 -0.3826 0.050 Uiso 1 1 calc R . .
H87C H 0.7114 0.0353 -0.3721 0.050 Uiso 1 1 calc R . .
C88 C 0.47749(10) -0.15466(13) -0.39692(14) 0.0282(5) Uani 1 1 d . . .
H88A H 0.4514 -0.1545 -0.3504 0.042 Uiso 1 1 calc R . .
H88B H 0.5067 -0.2004 -0.3900 0.042 Uiso 1 1 calc R . .
H88C H 0.4498 -0.1589 -0.4519 0.042 Uiso 1 1 calc R . .
C89 C 0.48796(11) 0.15277(13) -0.38044(15) 0.0305(5) Uani 1 1 d . . .
H89A H 0.5203 0.1939 -0.3638 0.046 Uiso 1 1 calc R . .
H89B H 0.4593 0.1493 -0.3370 0.046 Uiso 1 1 calc R . .
H89C H 0.4634 0.1670 -0.4356 0.046 Uiso 1 1 calc R . .
O91A O 0.84868(9) -0.08426(12) 0.53689(14) 0.0583(5) Uani 0.726(6) 1 d P A 1
C92A C 0.87903(15) -0.00514(18) 0.5510(2) 0.0559(8) Uani 0.726(6) 1 d P A 1
H92A H 0.9225 -0.0077 0.5352 0.067 Uiso 0.726(6) 1 calc PR A 1
H92B H 0.8545 0.0346 0.5132 0.067 Uiso 0.726(6) 1 calc PR A 1
C93A C 0.88279(16) 0.0215(2) 0.6390(2) 0.0438(11) Uani 0.726(6) 1 d P A 1
H93A H 0.9032 0.0743 0.6451 0.066 Uiso 0.726(6) 1 calc PR A 1
H93B H 0.9079 -0.0170 0.6767 0.066 Uiso 0.726(6) 1 calc PR A 1
H93C H 0.8398 0.0252 0.6547 0.066 Uiso 0.726(6) 1 calc PR A 1
O91B O 0.84868(9) -0.08426(12) 0.53689(14) 0.0583(5) Uani 0.274(6) 1 d P A 2
C92B C 0.87903(15) -0.00514(18) 0.5510(2) 0.0559(8) Uani 0.274(6) 1 d P A 2
H92C H 0.9116 -0.0056 0.5118 0.067 Uiso 0.274(6) 1 calc PR A 2
H92D H 0.9033 -0.0101 0.6090 0.067 Uiso 0.274(6) 1 calc PR A 2
C93B C 0.8564(4) 0.0845(7) 0.5479(8) 0.060(4) Uani 0.274(6) 1 d P A 2
H93D H 0.8932 0.1198 0.5628 0.091 Uiso 0.274(6) 1 calc PR A 2
H93E H 0.8262 0.0925 0.5889 0.091 Uiso 0.274(6) 1 calc PR A 2
H93F H 0.8355 0.0973 0.4902 0.091 Uiso 0.274(6) 1 calc PR A 2
H20 H 0.6491(12) -0.2148(17) 0.1600(16) 0.042(7) Uiso 1 1 d . . .
H30 H 0.5438(13) 0.1453(16) 0.1463(16) 0.045(7) Uiso 1 1 d . . .
H29 H 0.5386(13) -0.1304(17) 0.1421(17) 0.050(8) Uiso 1 1 d . . .
H39 H 0.6528(13) 0.2279(17) 0.1726(17) 0.050(8) Uiso 1 1 d . . .
H10 H 1.0304(14) -0.1496(18) 0.1101(18) 0.053(8) Uiso 1 1 d . . .
H9 H 1.0336(15) 0.131(2) 0.111(2) 0.068(10) Uiso 1 1 d . . .
H19 H 0.9304(13) -0.2368(17) 0.1365(17) 0.044(8) Uiso 1 1 d . . .
H40 H 0.9380(13) 0.2224(18) 0.1381(17) 0.051(8) Uiso 1 1 d . . .

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 0.0143(8) 0.0198(10) 0.0263(10) 0.0008(8) 0.0010(7) -0.0003(7)
C2 0.0120(8) 0.0193(10) 0.0285(11) -0.0001(8) -0.0015(8) -0.0005(7)
C3 0.0139(9) 0.0209(10) 0.0333(12) 0.0055(9) 0.0000(8) -0.0009(7)
C4 0.0149(9) 0.0272(11) 0.0279(11) 0.0005(9) 0.0044(8) 0.0008(8)
C5 0.0140(9) 0.0206(10) 0.0323(12) -0.0024(8) 0.0005(8) 0.0023(7)
C6 0.0133(9) 0.0191(10) 0.0286(11) 0.0013(8) 0.0000(8) -0.0005(7)
C7 0.0163(9) 0.0147(9) 0.0303(11) -0.0002(8) 0.0016(8) 0.0019(7)
C8 0.0209(10) 0.0190(10) 0.0300(11) 0.0009(8) -0.0007(8) 0.0009(8)
O9 0.0190(7) 0.0231(8) 0.0403(9) 0.0079(7) 0.0079(7) 0.0001(6)
O10 0.0200(7) 0.0222(7) 0.0379(9) -0.0037(6) 0.0096(6) 0.0002(6)
C11 0.0191(9) 0.0143(9) 0.0241(10) -0.0010(8) 0.0010(8) -0.0005(7)
C12 0.0169(9) 0.0141(9) 0.0271(11) 0.0025(8) -0.0003(8) 0.0000(7)
C13 0.0201(9) 0.0183(10) 0.0266(11) -0.0003(8) 0.0055(8) 0.0017(7)
C14 0.0242(10) 0.0180(10) 0.0235(10) -0.0028(8) 0.0015(8) -0.0014(8)
C15 0.0167(9) 0.0161(9) 0.0250(10) 0.0022(8) -0.0006(8) -0.0024(7)
C16 0.0175(9) 0.0130(9) 0.0244(10) 0.0019(7) 0.0019(8) 0.0021(7)
C17 0.0160(9) 0.0157(9) 0.0247(10) -0.0007(8) 0.0022(8) -0.0023(7)
C18 0.0216(10) 0.0217(10) 0.0271(11) -0.0001(8) 0.0032(8) 0.0000(8)
O19 0.0200(7) 0.0290(8) 0.0387(9) -0.0102(7) 0.0077(6) -0.0012(6)
O20 0.0173(7) 0.0234(7) 0.0297(8) -0.0069(6) -0.0002(6) -0.0027(6)
C21 0.0130(8) 0.0196(9) 0.0223(10) -0.0002(8) -0.0001(7) -0.0001(7)
C22 0.0144(9) 0.0184(9) 0.0221(10) -0.0010(8) 0.0032(7) 0.0006(7)
C23 0.0165(9) 0.0184(10) 0.0236(10) -0.0029(8) 0.0036(8) -0.0022(7)
C24 0.0141(8) 0.0222(10) 0.0237(10) -0.0011(8) -0.0010(7) 0.0001(7)
C25 0.0149(9) 0.0180(9) 0.0226(10) 0.0020(8) 0.0035(7) 0.0023(7)
C26 0.0145(9) 0.0190(9) 0.0218(10) -0.0012(8) 0.0031(7) -0.0012(7)
C27 0.0159(9) 0.0157(9) 0.0244(10) -0.0006(8) 0.0004(8) 0.0006(7)
C28 0.0236(10) 0.0199(10) 0.0261(11) -0.0017(8) 0.0020(8) -0.0013(8)
O29 0.0174(7) 0.0190(7) 0.0318(8) -0.0043(6) -0.0037(6) -0.0016(5)
O30 0.0167(7) 0.0179(7) 0.0317(8) 0.0028(6) -0.0033(6) 0.0013(5)
C31 0.0189(9) 0.0138(9) 0.0242(10) 0.0002(8) -0.0005(8) -0.0004(7)
C32 0.0175(9) 0.0126(9) 0.0249(10) -0.0030(8) -0.0007(8) -0.0014(7)
C33 0.0162(9) 0.0151(9) 0.0242(10) -0.0023(8) -0.0020(8) -0.0003(7)
C34 0.0245(10) 0.0166(9) 0.0222(10) 0.0009(8) 0.0011(8) 0.0009(8)
C35 0.0207(10) 0.0174(10) 0.0277(11) -0.0003(8) 0.0031(8) -0.0032(7)
C36 0.0178(9) 0.0147(9) 0.0255(10) -0.0022(8) -0.0012(8) -0.0015(7)
C37 0.0160(9) 0.0155(9) 0.0302(11) 0.0016(8) 0.0004(8) -0.0020(7)
C38 0.0196(10) 0.0203(10) 0.0333(12) 0.0006(9) -0.0031(9) -0.0013(8)
O39 0.0189(7) 0.0230(7) 0.0306(8) 0.0063(6) -0.0007(6) 0.0034(6)
O40 0.0206(7) 0.0267(8) 0.0373(9) 0.0099(7) 0.0068(6) 0.0009(6)
C41 0.0199(9) 0.0130(9) 0.0292(11) -0.0034(8) 0.0016(8) -0.0001(7)
C42 0.0214(10) 0.0308(12) 0.0289(12) -0.0032(9) 0.0034(9) 0.0011(8)
C43 0.0216(10) 0.0357(13) 0.0340(13) -0.0070(10) -0.0010(9) 0.0031(9)
N44 0.0203(8) 0.0236(9) 0.0424(11) -0.0049(8) 0.0040(8) 0.0010(7)
C45 0.0244(10) 0.0198(10) 0.0387(13) 0.0013(9) 0.0087(9) 0.0012(8)
C46 0.0237(10) 0.0175(10) 0.0297(11) 0.0023(8) 0.0021(9) -0.0010(8)
C47 0.0192(9) 0.0151(9) 0.0250(11) 0.0032(8) 0.0001(8) 0.0000(7)
C48 0.0249(10) 0.0209(10) 0.0261(11) -0.0012(8) 0.0024(8) -0.0010(8)
C49 0.0241(10) 0.0254(11) 0.0253(11) -0.0013(9) -0.0039(9) -0.0038(8)
N50 0.0187(8) 0.0252(9) 0.0297(10) 0.0010(8) -0.0010(7) -0.0008(7)
C51 0.0220(10) 0.0235(10) 0.0277(11) -0.0027(9) 0.0029(9) -0.0009(8)
C52 0.0223(10) 0.0218(10) 0.0248(11) -0.0027(8) -0.0019(8) -0.0036(8)
C61 0.0210(10) 0.0132(9) 0.0314(11) 0.0029(8) 0.0015(8) -0.0001(7)
C62 0.0252(10) 0.0272(11) 0.0318(12) -0.0011(9) 0.0032(9) -0.0014(9)
C63 0.0252(11) 0.0284(12) 0.0408(14) -0.0001(10) 0.0100(10) -0.0024(9)
N64 0.0202(9) 0.0266(10) 0.0497(12) 0.0075(9) 0.0058(8) -0.0013(7)
C65 0.0227(11) 0.0427(14) 0.0407(14) 0.0131(11) -0.0021(10) -0.0039(10)
C66 0.0200(10) 0.0372(13) 0.0328(12) 0.0076(10) 0.0021(9) -0.0019(9)
C67 0.0186(9) 0.0144(9) 0.0277(11) 0.0039(8) 0.0006(8) 0.0010(7)
C68 0.0233(10) 0.0188(10) 0.0289(11) -0.0010(8) 0.0046(8) 0.0025(8)
C69 0.0238(10) 0.0226(10) 0.0288(11) -0.0006(9) -0.0029(9) -0.0005(8)
N70 0.0193(8) 0.0215(9) 0.0303(10) 0.0027(7) -0.0002(7) 0.0018(7)
C71 0.0232(10) 0.0322(12) 0.0291(12) 0.0031(9) 0.0039(9) 0.0024(9)
C72 0.0235(10) 0.0277(11) 0.0255(11) 0.0001(9) -0.0018(8) -0.0025(8)
C81 0.0205(9) 0.0283(11) 0.0201(10) 0.0010(8) 0.0000(8) -0.0007(8)
C82 0.0266(10) 0.0209(10) 0.0237(11) 0.0019(8) -0.0004(8) 0.0045(8)
C83 0.0256(10) 0.0214(10) 0.0213(10) 0.0015(8) 0.0007(8) -0.0009(8)
C84 0.0188(9) 0.0260(11) 0.0219(10) -0.0002(8) 0.0022(8) 0.0000(8)
C85 0.0253(10) 0.0224(10) 0.0188(10) -0.0010(8) 0.0024(8) 0.0005(8)
C86 0.0244(10) 0.0222(10) 0.0220(10) 0.0002(8) 0.0012(8) -0.0036(8)
C87 0.0237(11) 0.0366(13) 0.0395(13) -0.0010(10) 0.0042(9) 0.0011(9)
C88 0.0304(11) 0.0216(10) 0.0320(12) 0.0025(9) 0.0028(9) -0.0024(9)
C89 0.0326(12) 0.0233(11) 0.0363(13) -0.0019(9) 0.0075(10) 0.0011(9)
O91A 0.0513(11) 0.0440(11) 0.0788(15) -0.0043(10) 0.0062(10) -0.0057(9)
C92A 0.0523(17) 0.0513(18) 0.068(2) 0.0014(15) 0.0223(15) -0.0042(13)
C93A 0.0226(16) 0.058(2) 0.052(2) -0.0182(18) 0.0087(15) -0.0067(15)
O91B 0.0513(11) 0.0440(11) 0.0788(15) -0.0043(10) 0.0062(10) -0.0057(9)
C92B 0.0523(17) 0.0513(18) 0.068(2) 0.0014(15) 0.0223(15) -0.0042(13)
C93B 0.029(5) 0.066(8) 0.089(9) -0.049(7) 0.023(5) -0.007(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 C6 1.393(3) . ?
C1 C2 1.394(3) . ?
C2 C3 1.389(3) . ?
C2 C37 1.524(3) . ?
C3 O9 1.380(2) . ?
C3 C4 1.384(3) . ?
C4 C5 1.385(3) . ?
C5 O10 1.379(2) . ?
C5 C6 1.389(3) . ?
C6 C7 1.520(3) . ?
C7 C8 1.527(3) . ?
C7 C12 1.528(2) . ?
C11 C12 1.389(3) . ?
C11 C16 1.393(2) . ?
C12 C13 1.392(3) . ?
C13 O19 1.376(2) . ?
C13 C14 1.383(3) . ?
C14 C15 1.386(3) . ?
C15 O20 1.371(2) . ?
C15 C16 1.396(3) . ?
C16 C17 1.523(3) . ?
C17 C22 1.521(3) . ?
C17 C18 1.527(3) . ?
C21 C26 1.388(3) . ?
C21 C22 1.390(3) . ?
C22 C23 1.391(3) . ?
C23 O29 1.375(2) . ?
C23 C24 1.385(3) . ?
C24 C25 1.385(3) . ?
C25 O30 1.374(2) . ?
C25 C26 1.392(3) . ?
C26 C27 1.523(3) . ?
C27 C32 1.518(3) . ?
C27 C28 1.529(3) . ?
C31 C36 1.385(3) . ?
C31 C32 1.388(2) . ?
C32 C33 1.397(3) . ?
C33 O39 1.376(2) . ?
C33 C34 1.377(3) . ?
C34 C35 1.389(3) . ?
C35 O40 1.372(2) . ?
C35 C36 1.392(3) . ?
C36 C37 1.525(2) . ?
C37 C38 1.527(3) . ?
C41 C46 1.385(3) . ?
C41 C42 1.387(3) . ?
C41 C47 1.481(3) . ?
C42 C43 1.383(3) . ?
C43 N44 1.333(3) . ?
N44 C45 1.329(3) . ?
C45 C46 1.381(3) . ?
C47 C52 1.386(3) . ?
C47 C48 1.388(3) . ?
C48 C49 1.375(3) . ?
C49 N50 1.332(3) . ?
N50 C51 1.340(3) . ?
C51 C52 1.378(3) . ?
C61 C66 1.382(3) . ?
C61 C62 1.385(3) . ?
C61 C67 1.488(3) . ?
C62 C63 1.383(3) . ?
C63 N64 1.329(3) . ?
N64 C65 1.329(3) . ?
C65 C66 1.385(3) . ?
C67 C72 1.386(3) . ?
C67 C68 1.389(3) . ?
C68 C69 1.373(3) . ?
C69 N70 1.331(3) . ?
N70 C71 1.332(3) . ?
C71 C72 1.382(3) . ?
C81 C86 1.387(3) . ?
C81 C82 1.390(3) . ?
C81 C87 1.509(3) . ?
C82 C83 1.393(3) . ?
C83 C84 1.386(3) . ?
C83 C88 1.505(3) . ?
C84 C85 1.388(3) . ?
C85 C86 1.389(3) . ?
C85 C89 1.506(3) . ?
O91A C92A 1.442(3) . ?
C92A C93A 1.422(5) . ?

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 123.45(19) . . ?
C3 C2 C1 117.14(18) . . ?
C3 C2 C37 120.55(18) . . ?
C1 C2 C37 122.31(18) . . ?
O9 C3 C4 120.09(19) . . ?
O9 C3 C2 118.65(18) . . ?
C4 C3 C2 121.25(18) . . ?
C3 C4 C5 119.72(19) . . ?
O10 C5 C4 119.82(18) . . ?
O10 C5 C6 118.67(18) . . ?
C4 C5 C6 121.49(19) . . ?
C5 C6 C1 116.90(18) . . ?
C5 C6 C7 121.03(18) . . ?
C1 C6 C7 122.06(18) . . ?
C6 C7 C8 112.67(16) . . ?
C6 C7 C12 110.82(15) . . ?
C8 C7 C12 112.82(16) . . ?
C12 C11 C16 123.95(18) . . ?
C11 C12 C13 117.17(17) . . ?
C11 C12 C7 121.29(17) . . ?
C13 C12 C7 121.51(17) . . ?
O19 C13 C14 116.15(17) . . ?
O19 C13 C12 123.01(17) . . ?
C14 C13 C12 120.82(18) . . ?
C13 C14 C15 120.40(18) . . ?
O20 C15 C14 115.94(17) . . ?
O20 C15 C16 123.13(17) . . ?
C14 C15 C16 120.88(17) . . ?
C11 C16 C15 116.67(17) . . ?
C11 C16 C17 121.80(17) . . ?
C15 C16 C17 121.53(16) . . ?
C22 C17 C16 111.97(15) . . ?
C22 C17 C18 112.66(16) . . ?
C16 C17 C18 112.68(15) . . ?
C26 C21 C22 123.74(17) . . ?
C21 C22 C23 117.12(17) . . ?
C21 C22 C17 121.92(16) . . ?
C23 C22 C17 120.96(16) . . ?
O29 C23 C24 120.53(17) . . ?
O29 C23 C22 118.49(17) . . ?
C24 C23 C22 120.97(17) . . ?
C23 C24 C25 120.07(18) . . ?
O30 C25 C24 120.29(16) . . ?
O30 C25 C26 118.72(17) . . ?
C24 C25 C26 121.00(17) . . ?
C21 C26 C25 117.07(17) . . ?
C21 C26 C27 121.77(16) . . ?
C25 C26 C27 121.14(16) . . ?
C32 C27 C26 110.73(15) . . ?
C32 C27 C28 112.76(15) . . ?
C26 C27 C28 112.43(16) . . ?
C36 C31 C32 124.26(18) . . ?
C31 C32 C33 116.62(17) . . ?
C31 C32 C27 121.65(17) . . ?
C33 C32 C27 121.73(16) . . ?
O39 C33 C34 116.20(17) . . ?
O39 C33 C32 122.77(17) . . ?
C34 C33 C32 120.97(17) . . ?
C33 C34 C35 120.55(18) . . ?
O40 C35 C34 116.00(17) . . ?
O40 C35 C36 123.47(17) . . ?
C34 C35 C36 120.48(18) . . ?
C31 C36 C35 117.07(17) . . ?
C31 C36 C37 121.26(17) . . ?
C35 C36 C37 121.67(17) . . ?
C2 C37 C36 111.10(15) . . ?
C2 C37 C38 112.74(16) . . ?
C36 C37 C38 112.86(16) . . ?
C46 C41 C42 117.46(18) . . ?
C46 C41 C47 120.65(18) . . ?
C42 C41 C47 121.85(18) . . ?
C43 C42 C41 119.2(2) . . ?
N44 C43 C42 123.3(2) . . ?
C45 N44 C43 117.27(18) . . ?
N44 C45 C46 123.4(2) . . ?
C45 C46 C41 119.4(2) . . ?
C52 C47 C48 117.16(17) . . ?
C52 C47 C41 121.49(17) . . ?
C48 C47 C41 121.31(18) . . ?
C49 C48 C47 119.46(19) . . ?
N50 C49 C48 123.69(19) . . ?
C49 N50 C51 116.81(17) . . ?
N50 C51 C52 123.29(19) . . ?
C51 C52 C47 119.56(18) . . ?
C66 C61 C62 117.47(18) . . ?
C66 C61 C67 121.50(19) . . ?
C62 C61 C67 120.98(18) . . ?
C63 C62 C61 119.2(2) . . ?
N64 C63 C62 123.4(2) . . ?
C63 N64 C65 117.34(18) . . ?
N64 C65 C66 123.2(2) . . ?
C61 C66 C65 119.4(2) . . ?
C72 C67 C68 116.82(17) . . ?
C72 C67 C61 123.00(18) . . ?
C68 C67 C61 120.18(18) . . ?
C69 C68 C67 119.56(19) . . ?
N70 C69 C68 123.96(19) . . ?
C69 N70 C71 116.48(17) . . ?
N70 C71 C72 123.7(2) . . ?
C71 C72 C67 119.45(19) . . ?
C86 C81 C82 118.55(18) . . ?
C86 C81 C87 120.57(18) . . ?
C82 C81 C87 120.88(18) . . ?
C81 C82 C83 121.29(18) . . ?
C84 C83 C82 118.67(18) . . ?
C84 C83 C88 120.83(18) . . ?
C82 C83 C88 120.50(18) . . ?
C83 C84 C85 121.31(18) . . ?
C84 C85 C86 118.73(18) . . ?
C84 C85 C89 121.06(18) . . ?
C86 C85 C89 120.20(18) . . ?
C81 C86 C85 121.45(18) . . ?
C93A C92A O91A 112.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.945
_diffrn_reflns_theta_full        27.90
_diffrn_measured_fraction_theta_full 0.945
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.066

#===END

data_nakamura9
_database_code_CSD               214036

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H34 N2 O4.50'
_chemical_formula_weight         530.62

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   Pbcn

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

_cell_length_a                   15.9821(16)
_cell_length_b                   14.3963(15)
_cell_length_c                   23.765(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5468.0(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    116(2)
_cell_measurement_reflns_used    312866
_cell_measurement_theta_min      1.90
_cell_measurement_theta_max      27.91

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2256
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      116(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            32866
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         27.91
_reflns_number_total             6439
_reflns_number_gt                4594
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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^)+(0.1048P)^2^+6.8270P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6439
_refine_ls_number_parameters     405
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_ref         0.2052
_refine_ls_wR_factor_gt          0.1871
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.979
_refine_ls_shift/su_max          0.011
_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 0.83715(13) 0.14276(16) 0.26446(9) 0.0208(5) Uani 1 1 d . . .
H1 H 0.8730 0.1933 0.2610 0.025 Uiso 1 1 calc R . .
C3 C 0.77173(15) 0.02932(19) 0.32218(10) 0.0284(6) Uani 1 1 d . . .
C4 C 0.73425(18) -0.0076(2) 0.27442(12) 0.0389(7) Uani 1 1 d . . .
H4 H 0.6992 -0.0589 0.2778 0.047 Uiso 1 1 calc R . .
C5 C 0.74837(16) 0.0310(2) 0.22186(11) 0.0345(6) Uani 1 1 d . . .
C6 C 0.80059(14) 0.10770(18) 0.21555(10) 0.0245(5) Uani 1 1 d . . .
C7 C 0.81774(14) 0.15184(18) 0.15850(10) 0.0251(5) Uani 1 1 d . . .
H7 H 0.7711 0.1346 0.1339 0.030 Uiso 1 1 calc R . .
C8 C 0.81899(17) 0.25810(19) 0.16128(11) 0.0313(6) Uani 1 1 d . . .
H8A H 0.8301 0.2828 0.1245 0.047 Uiso 1 1 calc R . .
H8B H 0.8620 0.2779 0.1868 0.047 Uiso 1 1 calc R . .
H8C H 0.7657 0.2802 0.1742 0.047 Uiso 1 1 calc R . .
O9 O 0.75386(11) -0.01407(14) 0.37214(8) 0.0337(5) Uani 1 1 d . . .
H9 H 0.7912 -0.0033 0.3949 0.051 Uiso 1 1 calc R . .
O10 O 0.70709(14) -0.00897(18) 0.17721(8) 0.0501(6) Uani 1 1 d . . .
H10 H 0.7362 -0.0052 0.1489 0.075 Uiso 1 1 calc R . .
C11 C 0.97620(14) 0.14855(16) 0.14120(9) 0.0205(5) Uani 1 1 d . . .
H11 H 0.9805 0.2016 0.1634 0.025 Uiso 1 1 calc R . .
C12 C 0.89684(14) 0.11104(17) 0.13226(9) 0.0219(5) Uani 1 1 d . . .
C13 C 0.89175(14) 0.03170(17) 0.09859(10) 0.0229(5) Uani 1 1 d . . .
C14 C 0.96294(15) -0.00603(17) 0.07429(10) 0.0243(5) Uani 1 1 d . . .
H14 H 0.9583 -0.0573 0.0507 0.029 Uiso 1 1 calc R . .
C15 C 1.04101(14) 0.03214(17) 0.08497(10) 0.0229(5) Uani 1 1 d . . .
C16 C 1.04943(14) 0.11111(16) 0.11880(9) 0.0204(5) Uani 1 1 d . . .
C17 C 1.13564(14) 0.15156(16) 0.13025(9) 0.0213(5) Uani 1 1 d . . .
H17 H 1.1707 0.1353 0.0979 0.026 Uiso 1 1 calc R . .
C18 C 1.13454(16) 0.25805(17) 0.13352(11) 0.0273(5) Uani 1 1 d . . .
H18A H 1.1902 0.2804 0.1405 0.041 Uiso 1 1 calc R . .
H18B H 1.0983 0.2773 0.1636 0.041 Uiso 1 1 calc R . .
H18C H 1.1144 0.2830 0.0986 0.041 Uiso 1 1 calc R . .
O19 O 0.81478(10) -0.00815(13) 0.08954(8) 0.0294(4) Uani 1 1 d . . .
H19 H 0.8210 -0.0622 0.0796 0.044 Uiso 1 1 calc R . .
O20 O 1.11136(10) -0.00649(12) 0.06151(8) 0.0281(4) Uani 1 1 d . . .
H20 H 1.1029 -0.0617 0.0551 0.042 Uiso 1 1 calc R . .
C2 C 0.82352(14) 0.10705(17) 0.31813(10) 0.0217(5) Uani 1 1 d . . .
C31 C 1.13157(14) -0.62099(18) -0.04486(10) 0.0254(5) Uani 1 1 d . . .
C32 C 1.09753(16) -0.66669(19) -0.09102(11) 0.0291(6) Uani 1 1 d . . .
H32 H 1.0642 -0.6344 -0.1164 0.035 Uiso 1 1 calc R . .
C33 C 1.11328(16) -0.7602(2) -0.09916(11) 0.0318(6) Uani 1 1 d . . .
H33 H 1.0894 -0.7893 -0.1302 0.038 Uiso 1 1 calc R . .
C35 C 1.19582(16) -0.76621(18) -0.02117(11) 0.0293(6) Uani 1 1 d . . .
H35 H 1.2302 -0.7999 0.0029 0.035 Uiso 1 1 calc R . .
N34 N 1.16102(13) -0.81078(15) -0.06474(9) 0.0291(5) Uani 1 1 d . . .
C36 C 1.18359(15) -0.67319(18) -0.00996(11) 0.0270(5) Uani 1 1 d . . .
H36 H 1.2099 -0.6455 0.0207 0.032 Uiso 1 1 calc R . .
C37 C 1.11292(15) -0.52295(18) -0.03444(11) 0.0277(5) Uani 1 1 d . . .
H37 H 1.0922 -0.4884 -0.0644 0.033 Uiso 1 1 calc R . .
C38 C 1.12314(15) -0.47909(18) 0.01430(11) 0.0270(5) Uani 1 1 d . . .
H38 H 1.1422 -0.5141 0.0446 0.032 Uiso 1 1 calc R . .
C39 C 1.10692(14) -0.38020(18) 0.02446(10) 0.0250(5) Uani 1 1 d . . .
C40 C 1.13096(16) -0.34025(19) 0.07557(10) 0.0287(5) Uani 1 1 d . . .
H40 H 1.1526 -0.3772 0.1041 0.034 Uiso 1 1 calc R . .
C41 C 1.12242(16) -0.24600(19) 0.08350(11) 0.0302(6) Uani 1 1 d . . .
H41 H 1.1392 -0.2209 0.1177 0.036 Uiso 1 1 calc R . .
N42 N 1.09126(13) -0.18863(15) 0.04456(9) 0.0293(5) Uani 1 1 d . . .
C43 C 1.06528(17) -0.22721(19) -0.00372(10) 0.0300(6) Uani 1 1 d . . .
H43 H 1.0418 -0.1887 -0.0309 0.036 Uiso 1 1 calc R . .
C44 C 1.07148(16) -0.32044(18) -0.01528(10) 0.0278(5) Uani 1 1 d . . .
H44 H 1.0522 -0.3437 -0.0494 0.033 Uiso 1 1 calc R . .
O61 O 0.0481(3) 0.4223(4) 0.3508(2) 0.0589(13) Uani 0.50 1 d P . .
H61 H 0.0942 0.4431 0.3424 0.088 Uiso 0.50 1 calc PR . .
C62 C -0.0130(4) 0.4580(5) 0.3132(3) 0.0500(16) Uani 0.50 1 d P . .
H62A H -0.0077 0.5250 0.3107 0.060 Uiso 0.50 1 calc PR . .
H62B H -0.0685 0.4436 0.3271 0.060 Uiso 0.50 1 calc PR . .
C63 C 0.0000 0.4112(4) 0.2500 0.0718(17) Uani 1 2 d S . .
H63A H -0.0406 0.4366 0.2245 0.108 Uiso 0.50 1 calc PR . .
H63B H -0.0072 0.3452 0.2524 0.108 Uiso 0.50 1 calc PR . .
H63C H 0.0553 0.4249 0.2365 0.108 Uiso 0.50 1 calc PR . .
C71 C 0.0174(5) 0.8672(4) 0.2496(7) 0.057(3) Uani 0.50 1 d PD . .
C72 C -0.0428(4) 0.8044(4) 0.2605(3) 0.0420(14) Uani 0.50 1 d PD . .
H72 H -0.0974 0.8246 0.2664 0.050 Uiso 0.50 1 calc PR . .
C73 C -0.0252(3) 0.7103(5) 0.2631(3) 0.0478(18) Uani 0.50 1 d PD . .
C74 C 0.0574(4) 0.6830(5) 0.2557(3) 0.0539(18) Uani 0.50 1 d PD . .
H74 H 0.0717 0.6207 0.2596 0.065 Uiso 0.50 1 calc PR . .
C75 C 0.1193(4) 0.7477(5) 0.2425(3) 0.059(2) Uani 0.50 1 d PD . .
H75 H 0.1737 0.7282 0.2350 0.071 Uiso 0.50 1 calc PR . .
C76 C 0.0992(4) 0.8411(5) 0.2407(3) 0.0531(19) Uani 0.50 1 d PD . .
H76 H 0.1402 0.8854 0.2337 0.064 Uiso 0.50 1 calc PR . .
C77 C 0.0000 0.9707(3) 0.2500 0.0699(16) Uani 1 2 d SD . .
H77A H -0.0593 0.9811 0.2479 0.105 Uiso 0.50 1 calc PR . .
H77B H 0.0268 0.9993 0.2182 0.105 Uiso 0.50 1 calc PR . .
H77C H 0.0215 0.9974 0.2841 0.105 Uiso 0.50 1 calc PR . .
C78 C -0.0928(5) 0.6407(7) 0.2758(4) 0.082(3) Uani 0.50 1 d PD . .
H78A H -0.1056 0.6061 0.2424 0.122 Uiso 0.50 1 calc PR . .
H78B H -0.1421 0.6727 0.2884 0.122 Uiso 0.50 1 calc PR . .
H78C H -0.0740 0.5991 0.3047 0.122 Uiso 0.50 1 calc PR . .

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 0.0140(10) 0.0238(11) 0.0246(12) -0.0025(9) 0.0008(8) 0.0022(9)
C3 0.0214(12) 0.0386(15) 0.0253(12) -0.0015(10) 0.0047(9) -0.0040(10)
C4 0.0316(14) 0.0512(18) 0.0338(15) -0.0065(13) 0.0048(11) -0.0209(13)
C5 0.0241(12) 0.0527(18) 0.0269(13) -0.0102(12) 0.0016(10) -0.0130(12)
C6 0.0162(11) 0.0331(13) 0.0241(12) -0.0042(10) 0.0013(9) 0.0026(9)
C7 0.0171(11) 0.0368(14) 0.0215(12) -0.0041(10) -0.0027(9) 0.0049(10)
C8 0.0289(13) 0.0398(15) 0.0253(13) 0.0009(11) -0.0018(10) 0.0140(11)
O9 0.0289(10) 0.0440(11) 0.0282(10) 0.0021(8) 0.0045(7) -0.0117(8)
O10 0.0407(12) 0.0806(16) 0.0291(11) -0.0142(11) 0.0025(9) -0.0346(12)
C11 0.0212(11) 0.0232(11) 0.0173(10) 0.0015(9) -0.0006(8) 0.0015(9)
C12 0.0209(11) 0.0283(12) 0.0166(11) 0.0005(9) -0.0015(8) 0.0043(9)
C13 0.0202(11) 0.0297(13) 0.0190(11) -0.0005(9) -0.0026(9) -0.0010(9)
C14 0.0274(12) 0.0255(12) 0.0201(11) -0.0057(9) 0.0002(9) -0.0007(10)
C15 0.0219(11) 0.0256(12) 0.0212(11) 0.0016(9) 0.0028(9) 0.0027(9)
C16 0.0195(11) 0.0241(12) 0.0175(10) 0.0032(9) -0.0003(8) 0.0001(9)
C17 0.0187(11) 0.0268(12) 0.0185(11) 0.0020(9) 0.0032(8) -0.0017(9)
C18 0.0291(13) 0.0256(12) 0.0272(13) 0.0053(10) 0.0035(10) -0.0045(10)
O19 0.0211(8) 0.0345(10) 0.0327(10) -0.0116(8) -0.0033(7) -0.0020(7)
O20 0.0234(9) 0.0302(9) 0.0306(9) -0.0085(8) 0.0056(7) 0.0025(7)
C2 0.0150(10) 0.0286(12) 0.0216(11) -0.0027(9) 0.0017(8) 0.0017(9)
C31 0.0168(11) 0.0327(13) 0.0267(12) 0.0026(10) 0.0026(9) -0.0034(10)
C32 0.0233(12) 0.0387(14) 0.0253(12) 0.0017(11) -0.0021(10) -0.0008(10)
C33 0.0268(13) 0.0397(15) 0.0289(13) -0.0046(11) 0.0004(10) -0.0071(11)
C35 0.0253(12) 0.0331(14) 0.0295(13) 0.0028(11) -0.0010(10) 0.0005(10)
N34 0.0241(10) 0.0324(11) 0.0308(11) -0.0004(9) 0.0036(9) -0.0046(9)
C36 0.0219(11) 0.0322(13) 0.0270(13) -0.0014(10) -0.0022(9) -0.0025(10)
C37 0.0224(12) 0.0336(14) 0.0272(13) 0.0046(10) -0.0008(9) 0.0012(10)
C38 0.0217(11) 0.0313(14) 0.0281(13) 0.0040(10) -0.0005(10) -0.0002(10)
C39 0.0189(11) 0.0312(13) 0.0249(12) 0.0033(10) 0.0031(9) -0.0012(9)
C40 0.0232(12) 0.0382(14) 0.0246(12) 0.0029(10) -0.0021(10) 0.0056(10)
C41 0.0244(12) 0.0408(15) 0.0253(13) -0.0030(11) -0.0025(10) 0.0044(11)
N42 0.0252(10) 0.0334(12) 0.0292(11) -0.0013(9) 0.0040(9) 0.0032(9)
C43 0.0340(14) 0.0335(14) 0.0226(12) 0.0049(10) 0.0011(10) 0.0036(11)
C44 0.0306(13) 0.0321(13) 0.0209(12) 0.0019(10) 0.0001(10) 0.0006(11)
O61 0.054(3) 0.069(3) 0.053(3) 0.008(2) -0.009(2) -0.006(3)
C62 0.051(4) 0.047(4) 0.051(4) 0.002(3) -0.010(3) -0.001(3)
C63 0.084(4) 0.054(3) 0.077(4) 0.000 -0.037(3) 0.000
C71 0.097(11) 0.051(3) 0.025(3) 0.003(5) -0.005(7) 0.008(4)
C72 0.036(3) 0.051(4) 0.039(3) -0.004(3) -0.004(3) 0.005(3)
C73 0.033(4) 0.070(5) 0.041(4) -0.019(3) 0.007(3) -0.022(3)
C74 0.063(5) 0.044(4) 0.055(5) 0.004(3) 0.007(4) 0.024(4)
C75 0.024(3) 0.116(7) 0.038(3) 0.003(4) 0.002(3) 0.025(4)
C76 0.041(4) 0.086(6) 0.032(3) 0.007(3) -0.005(3) -0.032(4)
C77 0.077(4) 0.050(3) 0.083(4) 0.000 0.019(3) 0.000
C78 0.069(6) 0.110(8) 0.065(5) -0.024(5) 0.014(4) -0.034(6)

_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 1.392(3) . ?
C1 C6 1.395(3) . ?
C3 O9 1.372(3) . ?
C3 C4 1.389(4) . ?
C3 C2 1.395(3) . ?
C4 C5 1.386(4) . ?
C5 O10 1.376(3) . ?
C5 C6 1.392(4) . ?
C6 C7 1.522(3) . ?
C7 C12 1.527(3) . ?
C7 C8 1.531(4) . ?
C11 C16 1.394(3) . ?
C11 C12 1.395(3) . ?
C12 C13 1.397(3) . ?
C13 O19 1.374(3) . ?
C13 C14 1.387(3) . ?
C14 C15 1.387(3) . ?
C15 O20 1.373(3) . ?
C15 C16 1.399(3) . ?
C16 C17 1.520(3) . ?
C17 C2 1.530(3) 3_755 ?
C17 C18 1.535(3) . ?
C2 C17 1.530(3) 3_755 ?
C31 C32 1.390(4) . ?
C31 C36 1.394(3) . ?
C31 C37 1.464(4) . ?
C32 C33 1.383(4) . ?
C33 N34 1.335(4) . ?
C35 N34 1.339(3) . ?
C35 C36 1.379(4) . ?
C37 C38 1.329(4) . ?
C38 C39 1.467(4) . ?
C39 C44 1.397(3) . ?
C39 C40 1.398(4) . ?
C40 C41 1.377(4) . ?
C41 N42 1.337(3) . ?
N42 C43 1.341(3) . ?
C43 C44 1.374(4) . ?
O61 C62 1.420(8) . ?
C62 C63 1.659(7) . ?
C71 C72 1.345(7) . ?
C71 C76 1.377(8) . ?
C71 C77 1.516(7) . ?
C72 C73 1.386(7) . ?
C73 C74 1.389(7) . ?
C73 C78 1.504(7) . ?
C74 C75 1.395(7) . ?
C75 C76 1.383(7) . ?

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 124.3(2) . . ?
O9 C3 C4 116.3(2) . . ?
O9 C3 C2 123.3(2) . . ?
C4 C3 C2 120.4(2) . . ?
C5 C4 C3 120.8(3) . . ?
O10 C5 C4 116.7(2) . . ?
O10 C5 C6 122.4(2) . . ?
C4 C5 C6 120.9(2) . . ?
C5 C6 C1 116.6(2) . . ?
C5 C6 C7 122.3(2) . . ?
C1 C6 C7 121.0(2) . . ?
C6 C7 C12 110.62(19) . . ?
C6 C7 C8 112.4(2) . . ?
C12 C7 C8 113.0(2) . . ?
C16 C11 C12 123.7(2) . . ?
C11 C12 C13 117.2(2) . . ?
C11 C12 C7 122.8(2) . . ?
C13 C12 C7 120.0(2) . . ?
O19 C13 C14 120.4(2) . . ?
O19 C13 C12 118.9(2) . . ?
C14 C13 C12 120.7(2) . . ?
C13 C14 C15 120.4(2) . . ?
O20 C15 C14 120.1(2) . . ?
O20 C15 C16 118.9(2) . . ?
C14 C15 C16 120.9(2) . . ?
C11 C16 C15 116.9(2) . . ?
C11 C16 C17 123.0(2) . . ?
C15 C16 C17 120.1(2) . . ?
C16 C17 C2 111.69(18) . 3_755 ?
C16 C17 C18 112.4(2) . . ?
C2 C17 C18 112.48(19) 3_755 . ?
C1 C2 C3 116.9(2) . . ?
C1 C2 C17 120.9(2) . 3_755 ?
C3 C2 C17 122.2(2) . 3_755 ?
C32 C31 C36 116.6(2) . . ?
C32 C31 C37 120.7(2) . . ?
C36 C31 C37 122.7(2) . . ?
C33 C32 C31 120.0(2) . . ?
N34 C33 C32 123.3(2) . . ?
N34 C35 C36 123.8(2) . . ?
C33 N34 C35 116.7(2) . . ?
C35 C36 C31 119.5(2) . . ?
C38 C37 C31 125.5(2) . . ?
C37 C38 C39 125.6(2) . . ?
C44 C39 C40 116.4(2) . . ?
C44 C39 C38 123.9(2) . . ?
C40 C39 C38 119.6(2) . . ?
C41 C40 C39 119.8(2) . . ?
N42 C41 C40 123.5(2) . . ?
C41 N42 C43 116.9(2) . . ?
N42 C43 C44 123.6(2) . . ?
C43 C44 C39 119.7(2) . . ?
O61 C62 C63 109.7(5) . . ?
C72 C71 C76 121.7(6) . . ?
C72 C71 C77 121.9(6) . . ?
C76 C71 C77 116.4(6) . . ?
C71 C72 C73 121.4(6) . . ?
C72 C73 C74 117.7(5) . . ?
C72 C73 C78 120.9(6) . . ?
C74 C73 C78 121.4(7) . . ?
C73 C74 C75 120.9(6) . . ?
C76 C75 C74 119.4(6) . . ?
C71 C76 C75 118.8(6) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.91
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.252
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.070

#===END

data_nakamura10
_database_code_CSD               214037

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C65 H64 N4 O8'
_chemical_formula_weight         1029.20

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                   11.7903(8)
_cell_length_b                   14.9265(10)
_cell_length_c                   15.6196(11)
_cell_angle_alpha                94.1590(10)
_cell_angle_beta                 92.5290(10)
_cell_angle_gamma                100.7580(10)
_cell_volume                     2688.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    116(2)
_cell_measurement_reflns_used    16647
_cell_measurement_theta_min      1.39
_cell_measurement_theta_max      27.89

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1092
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      116(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            16647
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0777
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.39
_diffrn_reflns_theta_max         27.89
_reflns_number_total             11743
_reflns_number_gt                8533
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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^)+(0.0453P)^2^+1.1749P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11743
_refine_ls_number_parameters     790
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0730
_refine_ls_wR_factor_ref         0.1614
_refine_ls_wR_factor_gt          0.1476
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.011
_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 0.9793(2) 0.22196(15) 0.53640(15) 0.0247(5) Uani 1 1 d . . .
H1 H 0.9970 0.1637 0.5345 0.030 Uiso 1 1 calc R . .
C2 C 0.8753(2) 0.23157(15) 0.49671(15) 0.0244(5) Uani 1 1 d . . .
C3 C 0.8519(2) 0.32033(16) 0.49944(16) 0.0257(5) Uani 1 1 d . . .
C4 C 0.9296(2) 0.39392(16) 0.53931(16) 0.0272(5) Uani 1 1 d . . .
H4 H 0.9130 0.4524 0.5393 0.033 Uiso 1 1 calc R . .
C5 C 1.0313(2) 0.38136(16) 0.57903(16) 0.0258(5) Uani 1 1 d . . .
C6 C 1.0590(2) 0.29364(15) 0.57884(15) 0.0235(5) Uani 1 1 d . . .
C7 C 1.1695(2) 0.27910(16) 0.62558(16) 0.0265(5) Uani 1 1 d . . .
H7 H 1.2276 0.3346 0.6215 0.032 Uiso 1 1 calc R . .
C8 C 1.2183(3) 0.19925(18) 0.58373(17) 0.0360(7) Uani 1 1 d . . .
H8A H 1.2878 0.1935 0.6156 0.054 Uiso 1 1 calc R . .
H8B H 1.2355 0.2107 0.5256 0.054 Uiso 1 1 calc R . .
H8C H 1.1623 0.1436 0.5839 0.054 Uiso 1 1 calc R . .
O9 O 0.75122(15) 0.33262(11) 0.45835(12) 0.0315(4) Uani 1 1 d . . .
H9 H 0.7305 0.3775 0.4815 0.047 Uiso 1 1 calc R . .
O10 O 1.10980(15) 0.45436(11) 0.61844(12) 0.0301(4) Uani 1 1 d . . .
H10 H 1.0757 0.4949 0.6351 0.045 Uiso 1 1 calc R . .
C11 C 1.1065(2) 0.18695(16) 0.75280(15) 0.0269(5) Uani 1 1 d . . .
H11 H 1.0838 0.1362 0.7135 0.032 Uiso 1 1 calc R . .
C12 C 1.1530(2) 0.27001(16) 0.72119(16) 0.0263(5) Uani 1 1 d . . .
C13 C 1.1860(2) 0.34548(16) 0.78160(17) 0.0297(6) Uani 1 1 d . . .
C14 C 1.1710(2) 0.33655(18) 0.86767(17) 0.0329(6) Uani 1 1 d . . .
H14 H 1.1935 0.3874 0.9069 0.040 Uiso 1 1 calc R . .
C15 C 1.1229(2) 0.25315(18) 0.89697(16) 0.0301(6) Uani 1 1 d . . .
C16 C 1.0918(2) 0.17501(16) 0.83929(15) 0.0256(5) Uani 1 1 d . . .
C17 C 1.0423(2) 0.08125(16) 0.86966(15) 0.0269(5) Uani 1 1 d . . .
H17 H 1.0650 0.0839 0.9311 0.032 Uiso 1 1 calc R . .
C18 C 1.0953(2) 0.00537(17) 0.82499(15) 0.0303(6) Uani 1 1 d . . .
H18A H 1.1781 0.0210 0.8325 0.045 Uiso 1 1 calc R . .
H18B H 1.0726 -0.0012 0.7647 0.045 Uiso 1 1 calc R . .
H18C H 1.0684 -0.0512 0.8497 0.045 Uiso 1 1 calc R . .
O19 O 1.23546(17) 0.43064(11) 0.75874(12) 0.0359(4) Uani 1 1 d . . .
H19 H 1.2020 0.4414 0.7146 0.054 Uiso 1 1 calc R . .
O20 O 1.10787(17) 0.25261(13) 0.98351(11) 0.0367(5) Uani 1 1 d . . .
H20 H 1.0528 0.2124 0.9919 0.055 Uiso 1 1 calc R . .
C21 C 0.8471(2) 0.01791(15) 0.78881(15) 0.0257(5) Uani 1 1 d . . .
H21 H 0.8867 -0.0057 0.7450 0.031 Uiso 1 1 calc R . .
C22 C 0.9115(2) 0.06267(16) 0.86184(15) 0.0266(5) Uani 1 1 d . . .
C23 C 0.8488(2) 0.09589(16) 0.92704(15) 0.0285(6) Uani 1 1 d . . .
C24 C 0.7308(2) 0.08838(16) 0.91736(15) 0.0299(6) Uani 1 1 d . . .
H24 H 0.6914 0.1129 0.9608 0.036 Uiso 1 1 calc R . .
C25 C 0.6699(2) 0.04425(16) 0.84291(15) 0.0276(6) Uani 1 1 d . . .
C26 C 0.7275(2) 0.00645(16) 0.77758(15) 0.0260(5) Uani 1 1 d . . .
C27 C 0.6596(2) -0.04318(16) 0.69667(15) 0.0266(5) Uani 1 1 d . . .
H27 H 0.5850 -0.0742 0.7152 0.032 Uiso 1 1 calc R . .
C28 C 0.7160(2) -0.11754(16) 0.65370(15) 0.0268(6) Uani 1 1 d . . .
H28A H 0.7315 -0.1586 0.6953 0.040 Uiso 1 1 calc R . .
H28B H 0.7873 -0.0898 0.6309 0.040 Uiso 1 1 calc R . .
H28C H 0.6649 -0.1509 0.6079 0.040 Uiso 1 1 calc R . .
O29 O 0.90862(16) 0.13587(13) 1.00217(11) 0.0342(4) Uani 1 1 d . . .
H29 H 0.8631 0.1510 1.0361 0.051 Uiso 1 1 calc R . .
O30 O 0.55208(16) 0.03544(13) 0.83356(11) 0.0350(4) Uani 1 1 d . . .
H30 H 0.5296 0.0654 0.8732 0.052 Uiso 1 1 calc R . .
C31 C 0.7148(2) 0.06032(15) 0.57725(15) 0.0242(5) Uani 1 1 d . . .
H31 H 0.7881 0.0461 0.5831 0.029 Uiso 1 1 calc R . .
C32 C 0.6325(2) 0.02351(15) 0.63231(15) 0.0243(5) Uani 1 1 d . . .
C33 C 0.5240(2) 0.04801(16) 0.62449(16) 0.0280(6) Uani 1 1 d . . .
C34 C 0.5013(2) 0.10551(16) 0.56283(16) 0.0284(6) Uani 1 1 d . . .
H34 H 0.4286 0.1209 0.5576 0.034 Uiso 1 1 calc R . .
C35 C 0.5854(2) 0.14013(16) 0.50908(15) 0.0269(5) Uani 1 1 d . . .
C36 C 0.6945(2) 0.11723(15) 0.51390(15) 0.0250(5) Uani 1 1 d . . .
C37 C 0.7883(2) 0.15154(15) 0.45309(15) 0.0259(5) Uani 1 1 d . . .
H37 H 0.7498 0.1751 0.4051 0.031 Uiso 1 1 calc R . .
C38 C 0.8440(2) 0.07417(16) 0.41451(16) 0.0294(6) Uani 1 1 d . . .
H38A H 0.7848 0.0260 0.3877 0.044 Uiso 1 1 calc R . .
H38B H 0.8857 0.0508 0.4593 0.044 Uiso 1 1 calc R . .
H38C H 0.8963 0.0972 0.3724 0.044 Uiso 1 1 calc R . .
O39 O 0.43590(16) 0.01661(13) 0.67606(11) 0.0357(5) Uani 1 1 d . . .
H39 H 0.4627 0.0148 0.7251 0.054 Uiso 1 1 calc R . .
O40 O 0.55589(16) 0.19858(12) 0.45024(12) 0.0328(4) Uani 1 1 d . . .
H40 H 0.6116 0.2395 0.4452 0.049 Uiso 1 1 calc R . .
C41 C 0.8641(2) 0.68552(17) 0.77617(15) 0.0266(5) Uani 1 1 d . . .
C42 C 0.9636(2) 0.72558(17) 0.73851(17) 0.0326(6) Uani 1 1 d . . .
H42 H 0.9880 0.7888 0.7445 0.039 Uiso 1 1 calc R . .
C43 C 1.0260(2) 0.67166(17) 0.69234(17) 0.0335(6) Uani 1 1 d . . .
H43 H 1.0927 0.7001 0.6682 0.040 Uiso 1 1 calc R . .
N44 N 0.99577(19) 0.58054(14) 0.68034(14) 0.0303(5) Uani 1 1 d . . .
C45 C 0.8998(2) 0.54231(17) 0.71593(17) 0.0327(6) Uani 1 1 d . . .
H45 H 0.8772 0.4790 0.7083 0.039 Uiso 1 1 calc R . .
C46 C 0.8318(2) 0.59074(17) 0.76336(16) 0.0299(6) Uani 1 1 d . . .
H46 H 0.7652 0.5605 0.7864 0.036 Uiso 1 1 calc R . .
C47 C 0.7998(2) 0.74212(17) 0.82862(15) 0.0276(6) Uani 1 1 d . . .
H47 H 0.8328 0.8038 0.8395 0.033 Uiso 1 1 calc R . .
C48 C 0.6993(2) 0.71382(17) 0.86200(14) 0.0242(5) Uani 1 1 d . . .
H48 H 0.6616 0.6542 0.8455 0.029 Uiso 1 1 calc R . .
C49 C 0.6418(2) 0.76784(17) 0.92252(14) 0.0236(5) Uani 1 1 d . . .
C50 C 0.5385(2) 0.72833(18) 0.95469(17) 0.0340(6) Uani 1 1 d . . .
H50 H 0.5042 0.6683 0.9364 0.041 Uiso 1 1 calc R . .
C51 C 0.4861(3) 0.77799(19) 1.01410(18) 0.0404(7) Uani 1 1 d . . .
H51 H 0.4159 0.7504 1.0340 0.049 Uiso 1 1 calc R . .
N52 N 0.53172(19) 0.86374(15) 1.04415(13) 0.0307(5) Uani 1 1 d . . .
C53 C 0.6303(2) 0.90161(17) 1.01237(16) 0.0288(6) Uani 1 1 d . . .
H53 H 0.6625 0.9618 1.0317 0.035 Uiso 1 1 calc R . .
C54 C 0.6876(2) 0.85801(17) 0.95324(16) 0.0288(6) Uani 1 1 d . . .
H54 H 0.7566 0.8882 0.9336 0.035 Uiso 1 1 calc R . .
C61 C 0.5509(2) 0.58562(17) 0.63466(16) 0.0295(6) Uani 1 1 d . . .
C62 C 0.6434(3) 0.61895(18) 0.58784(17) 0.0370(7) Uani 1 1 d . . .
H62 H 0.6676 0.6818 0.5867 0.044 Uiso 1 1 calc R . .
C63 C 0.7005(2) 0.55995(18) 0.54259(17) 0.0345(6) Uani 1 1 d . . .
H63 H 0.7624 0.5848 0.5113 0.041 Uiso 1 1 calc R . .
N64 N 0.67163(19) 0.46929(14) 0.54139(14) 0.0332(5) Uani 1 1 d . . .
C65 C 0.5836(3) 0.43675(19) 0.5867(2) 0.0455(8) Uani 1 1 d . . .
H65 H 0.5619 0.3736 0.5869 0.055 Uiso 1 1 calc R . .
C66 C 0.5213(3) 0.4910(2) 0.6341(2) 0.0442(7) Uani 1 1 d . . .
H66 H 0.4604 0.4642 0.6653 0.053 Uiso 1 1 calc R . .
C67 C 0.4893(2) 0.65018(17) 0.68193(16) 0.0307(6) Uani 1 1 d . . .
H67 H 0.5154 0.7125 0.6783 0.037 Uiso 1 1 calc R . .
C68 C 0.4010(2) 0.62546(18) 0.72834(16) 0.0306(6) Uani 1 1 d . . .
H68 H 0.3745 0.5630 0.7308 0.037 Uiso 1 1 calc R . .
C69 C 0.3398(2) 0.68819(17) 0.77706(15) 0.0285(6) Uani 1 1 d . . .
C70 C 0.2619(3) 0.65144(19) 0.83536(17) 0.0384(7) Uani 1 1 d . . .
H70 H 0.2471 0.5888 0.8409 0.046 Uiso 1 1 calc R . .
C71 C 0.2071(3) 0.70826(19) 0.88476(18) 0.0413(7) Uani 1 1 d . . .
H71 H 0.1562 0.6823 0.9240 0.050 Uiso 1 1 calc R . .
N72 N 0.2226(2) 0.79864(15) 0.87974(13) 0.0349(5) Uani 1 1 d . . .
C73 C 0.2952(2) 0.83379(18) 0.82261(16) 0.0322(6) Uani 1 1 d . . .
H73 H 0.3064 0.8965 0.8176 0.039 Uiso 1 1 calc R . .
C74 C 0.3550(2) 0.78252(18) 0.77014(16) 0.0305(6) Uani 1 1 d . . .
H74 H 0.4045 0.8103 0.7310 0.037 Uiso 1 1 calc R . .
C81 C 0.4498(4) 0.6951(3) 0.2045(3) 0.0286(12) Uani 0.499(3) 1 d PD A 1
C82 C 0.4345(6) 0.6213(4) 0.1417(4) 0.0342(14) Uani 0.499(3) 1 d PD A 1
H82 H 0.4986 0.5987 0.1237 0.041 Uiso 0.499(3) 1 calc PR A 1
C83 C 0.3264(7) 0.5817(5) 0.1063(4) 0.034(2) Uani 0.499(3) 1 d PD A 1
C84 C 0.2305(5) 0.6170(4) 0.1339(4) 0.0368(15) Uani 0.499(3) 1 d PD A 1
H84 H 0.1578 0.5895 0.1097 0.044 Uiso 0.499(3) 1 calc PR A 1
C85 C 0.2372(17) 0.6877(13) 0.1930(9) 0.030(3) Uani 0.499(3) 1 d PD A 1
C86 C 0.3530(4) 0.7270(3) 0.2309(3) 0.0274(12) Uani 0.499(3) 1 d PD A 1
H86 H 0.3618 0.7748 0.2738 0.033 Uiso 0.499(3) 1 calc PR A 1
C87 C 0.5680(5) 0.7398(4) 0.2401(4) 0.0479(17) Uani 0.499(3) 1 d PD A 1
H87A H 0.6184 0.7509 0.1939 0.072 Uiso 0.499(3) 1 calc PR A 1
H87B H 0.5972 0.7003 0.2779 0.072 Uiso 0.499(3) 1 calc PR A 1
H87C H 0.5644 0.7968 0.2716 0.072 Uiso 0.499(3) 1 calc PR A 1
C88 C 0.3119(8) 0.5046(4) 0.0352(4) 0.062(2) Uani 0.499(3) 1 d PD A 1
H88A H 0.3066 0.5292 -0.0197 0.093 Uiso 0.499(3) 1 calc PR A 1
H88B H 0.2427 0.4611 0.0422 0.093 Uiso 0.499(3) 1 calc PR A 1
H88C H 0.3774 0.4749 0.0380 0.093 Uiso 0.499(3) 1 calc PR A 1
C89 C 0.1387(5) 0.7237(4) 0.2292(4) 0.0464(17) Uani 0.499(3) 1 d PD A 1
H89A H 0.0681 0.6938 0.1982 0.070 Uiso 0.499(3) 1 calc PR A 1
H89B H 0.1497 0.7884 0.2239 0.070 Uiso 0.499(3) 1 calc PR A 1
H89C H 0.1348 0.7122 0.2887 0.070 Uiso 0.499(3) 1 calc PR A 1
C91 C 0.1731(4) 0.5715(3) 0.0790(3) 0.0311(13) Uani 0.501(3) 1 d PD A 2
C92 C 0.2825(6) 0.5491(4) 0.0746(4) 0.0279(13) Uani 0.501(3) 1 d PD A 2
H92 H 0.2948 0.5068 0.0309 0.034 Uiso 0.501(3) 1 calc PR A 2
C93 C 0.3728(6) 0.5873(5) 0.1325(5) 0.0281(17) Uani 0.501(3) 1 d PD A 2
C94 C 0.3536(5) 0.6511(3) 0.1977(3) 0.0311(13) Uani 0.501(3) 1 d PD A 2
H94 H 0.4148 0.6768 0.2367 0.037 Uiso 0.501(3) 1 calc PR A 2
C95 C 0.2516(17) 0.6773(12) 0.2069(8) 0.020(2) Uani 0.501(3) 1 d PD A 2
C96 C 0.1575(5) 0.6363(4) 0.1434(3) 0.0298(12) Uani 0.501(3) 1 d PD A 2
H96 H 0.0862 0.6541 0.1464 0.036 Uiso 0.501(3) 1 calc PR A 2
C97 C 0.0740(5) 0.5255(5) 0.0183(4) 0.0492(17) Uani 0.501(3) 1 d PD A 2
H97A H 0.1012 0.5164 -0.0381 0.074 Uiso 0.501(3) 1 calc PR A 2
H97B H 0.0165 0.5633 0.0162 0.074 Uiso 0.501(3) 1 calc PR A 2
H97C H 0.0407 0.4675 0.0379 0.074 Uiso 0.501(3) 1 calc PR A 2
C98 C 0.4904(5) 0.5596(4) 0.1281(4) 0.0408(14) Uani 0.501(3) 1 d PD A 2
H98A H 0.5032 0.5254 0.1762 0.061 Uiso 0.501(3) 1 calc PR A 2
H98B H 0.5497 0.6134 0.1297 0.061 Uiso 0.501(3) 1 calc PR A 2
H98C H 0.4923 0.5224 0.0756 0.061 Uiso 0.501(3) 1 calc PR A 2
C99 C 0.2276(6) 0.7455(4) 0.2744(3) 0.0407(15) Uani 0.501(3) 1 d PD A 2
H99A H 0.1839 0.7144 0.3175 0.061 Uiso 0.501(3) 1 calc PR A 2
H99B H 0.1841 0.7861 0.2490 0.061 Uiso 0.501(3) 1 calc PR A 2
H99C H 0.2994 0.7800 0.3003 0.061 Uiso 0.501(3) 1 calc PR A 2

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 0.0358(14) 0.0123(11) 0.0286(13) 0.0011(9) 0.0135(11) 0.0089(10)
C2 0.0317(14) 0.0145(11) 0.0280(13) -0.0002(9) 0.0096(11) 0.0062(10)
C3 0.0295(14) 0.0184(12) 0.0310(13) -0.0001(10) 0.0055(11) 0.0093(10)
C4 0.0332(14) 0.0141(11) 0.0374(14) 0.0006(10) 0.0093(11) 0.0116(10)
C5 0.0306(14) 0.0157(11) 0.0313(13) -0.0024(10) 0.0122(11) 0.0046(10)
C6 0.0314(14) 0.0137(11) 0.0277(12) 0.0018(9) 0.0121(10) 0.0079(9)
C7 0.0339(14) 0.0197(12) 0.0299(13) 0.0031(10) 0.0120(11) 0.0126(10)
C8 0.0523(18) 0.0304(14) 0.0342(14) 0.0051(12) 0.0200(13) 0.0255(13)
O9 0.0349(10) 0.0175(9) 0.0435(11) -0.0042(8) 0.0017(8) 0.0111(7)
O10 0.0306(10) 0.0161(9) 0.0446(11) -0.0039(8) 0.0065(8) 0.0083(7)
C11 0.0371(15) 0.0187(12) 0.0264(13) -0.0048(10) 0.0078(11) 0.0104(10)
C12 0.0298(14) 0.0219(12) 0.0299(13) -0.0001(10) 0.0086(11) 0.0113(10)
C13 0.0298(14) 0.0193(12) 0.0407(15) -0.0020(11) 0.0093(12) 0.0066(10)
C14 0.0348(15) 0.0241(13) 0.0380(15) -0.0108(11) 0.0051(12) 0.0055(11)
C15 0.0346(15) 0.0327(14) 0.0237(13) -0.0069(11) 0.0041(11) 0.0114(11)
C16 0.0318(14) 0.0203(12) 0.0264(13) -0.0030(10) 0.0068(10) 0.0100(10)
C17 0.0409(15) 0.0218(12) 0.0193(12) -0.0017(10) 0.0044(11) 0.0101(11)
C18 0.0470(17) 0.0232(13) 0.0238(13) -0.0009(10) 0.0070(12) 0.0148(11)
O19 0.0401(12) 0.0183(9) 0.0473(12) 0.0004(8) 0.0016(9) 0.0010(8)
O20 0.0470(13) 0.0366(11) 0.0240(9) -0.0095(8) 0.0040(8) 0.0058(9)
C21 0.0419(15) 0.0154(11) 0.0208(12) -0.0006(9) 0.0131(11) 0.0058(10)
C22 0.0418(15) 0.0176(12) 0.0216(12) 0.0020(9) 0.0095(11) 0.0066(10)
C23 0.0445(16) 0.0208(12) 0.0191(12) -0.0022(10) 0.0079(11) 0.0038(11)
C24 0.0431(16) 0.0231(13) 0.0231(12) -0.0058(10) 0.0146(11) 0.0049(11)
C25 0.0373(15) 0.0196(12) 0.0262(13) -0.0003(10) 0.0131(11) 0.0046(10)
C26 0.0406(15) 0.0157(12) 0.0217(12) 0.0010(9) 0.0112(11) 0.0034(10)
C27 0.0367(15) 0.0182(12) 0.0244(12) -0.0007(10) 0.0110(11) 0.0032(10)
C28 0.0431(16) 0.0149(11) 0.0222(12) -0.0010(9) 0.0040(11) 0.0052(10)
O29 0.0450(12) 0.0355(11) 0.0210(9) -0.0090(8) 0.0085(8) 0.0072(9)
O30 0.0401(11) 0.0356(11) 0.0283(10) -0.0084(8) 0.0135(8) 0.0064(8)
C31 0.0289(13) 0.0151(11) 0.0292(13) -0.0045(9) 0.0067(10) 0.0071(9)
C32 0.0348(14) 0.0147(11) 0.0230(12) -0.0059(9) 0.0064(10) 0.0050(10)
C33 0.0335(14) 0.0221(13) 0.0262(13) -0.0084(10) 0.0089(11) 0.0019(10)
C34 0.0311(14) 0.0216(13) 0.0324(14) -0.0091(10) 0.0043(11) 0.0084(10)
C35 0.0390(15) 0.0164(12) 0.0262(13) -0.0052(10) 0.0030(11) 0.0098(10)
C36 0.0362(14) 0.0116(11) 0.0270(13) -0.0046(9) 0.0062(11) 0.0058(10)
C37 0.0364(15) 0.0151(11) 0.0269(13) -0.0015(10) 0.0048(11) 0.0077(10)
C38 0.0386(15) 0.0191(12) 0.0310(13) -0.0026(10) 0.0123(11) 0.0066(11)
O39 0.0338(11) 0.0398(11) 0.0320(10) -0.0040(9) 0.0123(8) 0.0035(8)
O40 0.0376(11) 0.0237(10) 0.0381(10) 0.0015(8) 0.0001(9) 0.0090(8)
C41 0.0355(15) 0.0235(13) 0.0235(12) 0.0026(10) 0.0031(11) 0.0123(11)
C42 0.0397(16) 0.0174(12) 0.0427(15) 0.0006(11) 0.0127(13) 0.0087(11)
C43 0.0358(15) 0.0240(13) 0.0413(15) 0.0002(11) 0.0121(12) 0.0061(11)
N44 0.0361(13) 0.0213(11) 0.0349(12) -0.0015(9) 0.0049(10) 0.0098(9)
C45 0.0474(17) 0.0174(12) 0.0353(14) 0.0012(11) 0.0106(13) 0.0097(11)
C46 0.0379(15) 0.0219(13) 0.0309(13) 0.0031(10) 0.0129(12) 0.0057(11)
C47 0.0368(15) 0.0222(13) 0.0257(13) 0.0015(10) 0.0032(11) 0.0100(11)
C48 0.0312(14) 0.0227(12) 0.0192(11) -0.0005(9) -0.0015(10) 0.0083(10)
C49 0.0288(13) 0.0279(13) 0.0151(11) 0.0004(9) -0.0012(10) 0.0089(10)
C50 0.0374(16) 0.0253(14) 0.0374(15) -0.0055(11) 0.0078(12) 0.0026(11)
C51 0.0441(17) 0.0319(15) 0.0444(17) -0.0002(13) 0.0229(14) 0.0013(13)
N52 0.0396(13) 0.0294(12) 0.0243(11) 0.0004(9) 0.0098(10) 0.0085(10)
C53 0.0329(15) 0.0257(13) 0.0276(13) -0.0020(10) 0.0036(11) 0.0061(11)
C54 0.0278(14) 0.0278(14) 0.0315(14) 0.0006(11) 0.0053(11) 0.0072(11)
C61 0.0358(15) 0.0251(13) 0.0277(13) -0.0046(10) -0.0017(11) 0.0090(11)
C62 0.0535(19) 0.0211(13) 0.0394(15) 0.0031(11) 0.0093(14) 0.0127(12)
C63 0.0428(17) 0.0255(14) 0.0386(15) 0.0044(11) 0.0114(13) 0.0125(12)
N64 0.0329(13) 0.0251(12) 0.0432(13) -0.0031(10) 0.0042(10) 0.0110(9)
C65 0.0439(18) 0.0212(14) 0.069(2) -0.0049(14) 0.0157(16) 0.0013(12)
C66 0.0351(17) 0.0379(17) 0.0591(19) 0.0005(14) 0.0190(15) 0.0034(13)
C67 0.0387(16) 0.0203(13) 0.0318(14) -0.0008(10) -0.0001(12) 0.0035(11)
C68 0.0353(15) 0.0259(13) 0.0282(13) -0.0043(11) 0.0001(11) 0.0028(11)
C69 0.0359(15) 0.0275(13) 0.0219(12) -0.0077(10) -0.0037(11) 0.0104(11)
C70 0.0562(19) 0.0252(14) 0.0350(15) 0.0019(12) 0.0112(14) 0.0088(13)
C71 0.061(2) 0.0313(15) 0.0344(15) 0.0057(12) 0.0200(14) 0.0119(14)
N72 0.0531(15) 0.0291(12) 0.0246(11) -0.0045(9) 0.0105(10) 0.0140(10)
C73 0.0460(17) 0.0212(13) 0.0298(14) -0.0015(11) 0.0073(12) 0.0073(11)
C74 0.0342(15) 0.0313(14) 0.0255(13) 0.0003(11) 0.0063(11) 0.0050(11)
C81 0.031(3) 0.027(3) 0.028(3) -0.005(2) -0.006(2) 0.009(2)
C82 0.041(4) 0.032(4) 0.030(3) -0.002(3) 0.000(3) 0.011(3)
C83 0.055(7) 0.019(3) 0.020(4) -0.005(3) -0.005(4) -0.006(4)
C84 0.035(4) 0.029(3) 0.040(3) 0.013(3) -0.019(3) -0.010(3)
C85 0.026(5) 0.029(5) 0.039(7) 0.021(4) -0.013(4) 0.009(3)
C86 0.030(3) 0.022(3) 0.030(3) -0.006(2) -0.004(2) 0.009(2)
C87 0.023(3) 0.051(4) 0.068(4) -0.018(3) -0.015(3) 0.014(3)
C88 0.110(7) 0.030(4) 0.035(4) -0.006(3) -0.013(4) -0.010(4)
C89 0.022(3) 0.044(4) 0.078(5) 0.019(3) -0.002(3) 0.014(3)
C91 0.033(3) 0.029(3) 0.029(3) 0.000(2) -0.004(2) 0.003(2)
C92 0.040(4) 0.020(3) 0.023(3) -0.007(2) 0.002(3) 0.006(3)
C93 0.027(5) 0.026(4) 0.029(4) -0.001(3) 0.001(3) 0.001(3)
C94 0.038(3) 0.026(3) 0.025(3) 0.001(2) -0.005(2) -0.004(2)
C95 0.030(6) 0.021(5) 0.010(3) 0.002(4) -0.006(4) 0.012(3)
C96 0.028(3) 0.034(3) 0.028(3) 0.003(2) -0.001(2) 0.008(2)
C97 0.038(4) 0.059(4) 0.048(4) -0.007(3) -0.011(3) 0.009(3)
C98 0.034(3) 0.041(3) 0.048(4) 0.004(3) -0.002(3) 0.011(3)
C99 0.065(4) 0.027(3) 0.032(3) -0.001(2) 0.011(3) 0.013(3)

_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 1.385(3) . ?
C1 C6 1.391(3) . ?
C2 C3 1.401(3) . ?
C2 C37 1.519(3) . ?
C3 O9 1.373(3) . ?
C3 C4 1.381(3) . ?
C4 C5 1.376(3) . ?
C5 O10 1.378(3) . ?
C5 C6 1.407(3) . ?
C6 C7 1.523(3) . ?
C7 C12 1.527(3) . ?
C7 C8 1.535(3) . ?
C11 C16 1.390(3) . ?
C11 C12 1.393(3) . ?
C12 C13 1.400(3) . ?
C13 O19 1.375(3) . ?
C13 C14 1.376(4) . ?
C14 C15 1.387(4) . ?
C15 O20 1.371(3) . ?
C15 C16 1.402(3) . ?
C16 C17 1.530(3) . ?
C17 C22 1.514(4) . ?
C17 C18 1.532(3) . ?
C21 C26 1.390(4) . ?
C21 C22 1.396(3) . ?
C22 C23 1.400(3) . ?
C23 C24 1.375(4) . ?
C23 O29 1.378(3) . ?
C24 C25 1.393(3) . ?
C25 O30 1.371(3) . ?
C25 C26 1.393(3) . ?
C26 C27 1.530(3) . ?
C27 C28 1.527(3) . ?
C27 C32 1.529(3) . ?
C31 C32 1.388(3) . ?
C31 C36 1.391(3) . ?
C32 C33 1.398(4) . ?
C33 O39 1.376(3) . ?
C33 C34 1.385(4) . ?
C34 C35 1.378(3) . ?
C35 O40 1.389(3) . ?
C35 C36 1.392(3) . ?
C36 C37 1.530(3) . ?
C37 C38 1.531(3) . ?
C41 C42 1.389(4) . ?
C41 C46 1.392(3) . ?
C41 C47 1.468(3) . ?
C42 C43 1.376(3) . ?
C43 N44 1.337(3) . ?
N44 C45 1.333(3) . ?
C45 C46 1.381(3) . ?
C47 C48 1.325(3) . ?
C48 C49 1.468(3) . ?
C49 C50 1.383(3) . ?
C49 C54 1.395(3) . ?
C50 C51 1.383(4) . ?
C51 N52 1.335(3) . ?
N52 C53 1.328(3) . ?
C53 C54 1.365(3) . ?
C61 C62 1.375(4) . ?
C61 C66 1.390(4) . ?
C61 C67 1.486(4) . ?
C62 C63 1.379(4) . ?
C63 N64 1.331(3) . ?
N64 C65 1.320(4) . ?
C65 C66 1.387(4) . ?
C67 C68 1.307(4) . ?
C68 C69 1.474(3) . ?
C69 C70 1.390(4) . ?
C69 C74 1.399(4) . ?
C70 C71 1.374(4) . ?
C71 N72 1.336(3) . ?
N72 C73 1.331(3) . ?
C73 C74 1.385(3) . ?
C81 C86 1.384(7) . ?
C81 C82 1.401(7) . ?
C81 C87 1.492(7) . ?
C82 C83 1.374(9) . ?
C83 C84 1.405(9) . ?
C83 C88 1.521(8) . ?
C84 C85 1.338(15) . ?
C85 C86 1.46(2) . ?
C85 C89 1.484(12) . ?
C91 C96 1.387(7) . ?
C91 C92 1.395(7) . ?
C91 C97 1.498(7) . ?
C92 C93 1.375(8) . ?
C93 C94 1.398(8) . ?
C93 C98 1.521(8) . ?
C94 C95 1.343(14) . ?
C95 C96 1.47(2) . ?
C95 C99 1.485(10) . ?

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 124.4(2) . . ?
C1 C2 C3 116.5(2) . . ?
C1 C2 C37 123.2(2) . . ?
C3 C2 C37 120.3(2) . . ?
O9 C3 C4 120.8(2) . . ?
O9 C3 C2 118.0(2) . . ?
C4 C3 C2 121.2(2) . . ?
C5 C4 C3 120.6(2) . . ?
C4 C5 O10 121.0(2) . . ?
C4 C5 C6 120.7(2) . . ?
O10 C5 C6 118.2(2) . . ?
C1 C6 C5 116.6(2) . . ?
C1 C6 C7 122.5(2) . . ?
C5 C6 C7 120.8(2) . . ?
C6 C7 C12 111.25(19) . . ?
C6 C7 C8 113.1(2) . . ?
C12 C7 C8 111.9(2) . . ?
C16 C11 C12 124.2(2) . . ?
C11 C12 C13 116.8(2) . . ?
C11 C12 C7 122.2(2) . . ?
C13 C12 C7 121.0(2) . . ?
O19 C13 C14 117.1(2) . . ?
O19 C13 C12 122.4(2) . . ?
C14 C13 C12 120.6(2) . . ?
C13 C14 C15 121.2(2) . . ?
O20 C15 C14 116.4(2) . . ?
O20 C15 C16 123.3(2) . . ?
C14 C15 C16 120.3(2) . . ?
C11 C16 C15 116.8(2) . . ?
C11 C16 C17 121.4(2) . . ?
C15 C16 C17 121.8(2) . . ?
C22 C17 C16 110.8(2) . . ?
C22 C17 C18 113.5(2) . . ?
C16 C17 C18 111.7(2) . . ?
C26 C21 C22 124.0(2) . . ?
C21 C22 C23 116.3(2) . . ?
C21 C22 C17 123.1(2) . . ?
C23 C22 C17 120.4(2) . . ?
C24 C23 O29 120.5(2) . . ?
C24 C23 C22 121.4(2) . . ?
O29 C23 C22 118.1(2) . . ?
C23 C24 C25 120.4(2) . . ?
O30 C25 C24 120.6(2) . . ?
O30 C25 C26 118.9(2) . . ?
C24 C25 C26 120.5(3) . . ?
C21 C26 C25 117.2(2) . . ?
C21 C26 C27 122.7(2) . . ?
C25 C26 C27 120.1(2) . . ?
C28 C27 C32 111.19(19) . . ?
C28 C27 C26 113.7(2) . . ?
C32 C27 C26 112.02(19) . . ?
C32 C31 C36 124.1(2) . . ?
C31 C32 C33 117.2(2) . . ?
C31 C32 C27 120.9(2) . . ?
C33 C32 C27 121.9(2) . . ?
O39 C33 C34 117.3(2) . . ?
O39 C33 C32 122.5(2) . . ?
C34 C33 C32 120.2(2) . . ?
C35 C34 C33 120.7(2) . . ?
C34 C35 O40 116.9(2) . . ?
C34 C35 C36 121.3(2) . . ?
O40 C35 C36 121.9(2) . . ?
C31 C36 C35 116.5(2) . . ?
C31 C36 C37 120.9(2) . . ?
C35 C36 C37 122.6(2) . . ?
C2 C37 C36 110.71(19) . . ?
C2 C37 C38 113.5(2) . . ?
C36 C37 C38 112.13(19) . . ?
C42 C41 C46 116.9(2) . . ?
C42 C41 C47 120.3(2) . . ?
C46 C41 C47 122.8(2) . . ?
C43 C42 C41 119.9(2) . . ?
N44 C43 C42 123.4(3) . . ?
C45 N44 C43 116.6(2) . . ?
N44 C45 C46 124.1(2) . . ?
C45 C46 C41 119.0(2) . . ?
C48 C47 C41 126.3(2) . . ?
C47 C48 C49 126.1(2) . . ?
C50 C49 C54 116.5(2) . . ?
C50 C49 C48 119.9(2) . . ?
C54 C49 C48 123.6(2) . . ?
C49 C50 C51 120.1(2) . . ?
N52 C51 C50 123.0(3) . . ?
C53 N52 C51 116.7(2) . . ?
N52 C53 C54 124.3(2) . . ?
C53 C54 C49 119.5(2) . . ?
C62 C61 C66 116.2(2) . . ?
C62 C61 C67 119.8(2) . . ?
C66 C61 C67 124.0(2) . . ?
C61 C62 C63 120.5(3) . . ?
N64 C63 C62 123.4(3) . . ?
C65 N64 C63 116.5(2) . . ?
N64 C65 C66 124.0(3) . . ?
C65 C66 C61 119.4(3) . . ?
C68 C67 C61 124.5(2) . . ?
C67 C68 C69 125.5(3) . . ?
C70 C69 C74 117.1(2) . . ?
C70 C69 C68 117.8(2) . . ?
C74 C69 C68 125.1(2) . . ?
C71 C70 C69 119.6(3) . . ?
N72 C71 C70 123.8(3) . . ?
C73 N72 C71 116.8(2) . . ?
N72 C73 C74 123.9(2) . . ?
C73 C74 C69 118.9(2) . . ?
C86 C81 C82 118.3(5) . . ?
C86 C81 C87 121.0(5) . . ?
C82 C81 C87 120.7(5) . . ?
C83 C82 C81 121.2(6) . . ?
C82 C83 C84 118.7(7) . . ?
C82 C83 C88 120.5(7) . . ?
C84 C83 C88 120.7(7) . . ?
C85 C84 C83 124.2(9) . . ?
C84 C85 C86 115.9(9) . . ?
C84 C85 C89 126.6(17) . . ?
C86 C85 C89 117.3(11) . . ?
C81 C86 C85 121.7(6) . . ?
C96 C91 C92 117.8(5) . . ?
C96 C91 C97 120.5(5) . . ?
C92 C91 C97 121.6(5) . . ?
C93 C92 C91 122.4(5) . . ?
C92 C93 C94 118.4(6) . . ?
C92 C93 C98 121.4(6) . . ?
C94 C93 C98 120.2(6) . . ?
C95 C94 C93 123.6(8) . . ?
C94 C95 C96 116.7(7) . . ?
C94 C95 C99 125.4(14) . . ?
C96 C95 C99 117.9(10) . . ?
C91 C96 C95 121.1(6) . . ?

_diffrn_measured_fraction_theta_max 0.913
_diffrn_reflns_theta_full        27.89
_diffrn_measured_fraction_theta_full 0.913
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.051

#===END

data_nakamura11
_database_code_CSD               214040

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H50 N3 O8'
_chemical_formula_weight         965.05

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                   10.3752(5)
_cell_length_b                   12.2621(6)
_cell_length_c                   20.1337(10)
_cell_angle_alpha                95.1810(10)
_cell_angle_beta                 103.9480(10)
_cell_angle_gamma                94.1660(10)
_cell_volume                     2463.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    116(2)
_cell_measurement_reflns_used    15372
_cell_measurement_theta_min      1.68
_cell_measurement_theta_max      27.89

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1014
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      116(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            15372
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         27.89
_reflns_number_total             10741
_reflns_number_gt                8956
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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^)+(0.0564P)^2^+0.6303P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10741
_refine_ls_number_parameters     690
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1354
_refine_ls_wR_factor_gt          0.1272
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.003

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 0.43667(17) 0.62608(14) -0.26850(9) 0.0176(3) Uani 1 1 d . . .
H1 H 0.3724 0.6743 -0.2816 0.021 Uiso 1 1 calc R . .
C2 C 0.50819(16) 0.63656(14) -0.19954(9) 0.0166(3) Uani 1 1 d . . .
C3 C 0.60329(17) 0.56205(14) -0.18169(9) 0.0179(3) Uani 1 1 d . . .
C4 C 0.62652(17) 0.48280(14) -0.22977(9) 0.0201(4) Uani 1 1 d . . .
H4 H 0.6915 0.4352 -0.2166 0.024 Uiso 1 1 calc R . .
C5 C 0.55245(17) 0.47448(14) -0.29787(9) 0.0183(3) Uani 1 1 d . . .
C6 C 0.45596(16) 0.54760(13) -0.31891(9) 0.0171(3) Uani 1 1 d . . .
C7 C 0.37626(17) 0.53900(14) -0.39376(9) 0.0191(4) Uani 1 1 d . . .
H7 H 0.4361 0.5161 -0.4222 0.023 Uiso 1 1 calc R . .
C8 C 0.32817(18) 0.64845(15) -0.41647(9) 0.0229(4) Uani 1 1 d . . .
H8A H 0.2789 0.6373 -0.4639 0.034 Uiso 1 1 calc R . .
H8B H 0.4038 0.7013 -0.4113 0.034 Uiso 1 1 calc R . .
H8C H 0.2717 0.6752 -0.3885 0.034 Uiso 1 1 calc R . .
O9 O 0.68095(12) 0.56563(11) -0.11473(6) 0.0225(3) Uani 1 1 d . . .
O10 O 0.58150(13) 0.39321(11) -0.34192(7) 0.0252(3) Uani 1 1 d . . .
C11 C 0.14682(17) 0.46291(14) -0.38341(9) 0.0193(4) Uani 1 1 d . . .
H11 H 0.1446 0.5281 -0.3564 0.023 Uiso 1 1 calc R . .
C12 C 0.26009(17) 0.44880(14) -0.40792(9) 0.0185(3) Uani 1 1 d . . .
C13 C 0.26434(17) 0.34798(14) -0.44536(8) 0.0183(3) Uani 1 1 d . . .
C14 C 0.15781(18) 0.26660(14) -0.45902(9) 0.0206(4) Uani 1 1 d . . .
H14 H 0.1625 0.1995 -0.4834 0.025 Uiso 1 1 calc R . .
C15 C 0.04419(18) 0.28567(14) -0.43618(9) 0.0194(4) Uani 1 1 d . . .
C16 C 0.03684(17) 0.38448(14) -0.39720(9) 0.0187(3) Uani 1 1 d . . .
C17 C -0.08572(17) 0.40400(14) -0.37006(9) 0.0190(4) Uani 1 1 d . . .
H17 H -0.1554 0.3454 -0.3935 0.023 Uiso 1 1 calc R . .
C18 C -0.14028(18) 0.51297(15) -0.38816(9) 0.0239(4) Uani 1 1 d . . .
H18A H -0.2172 0.5220 -0.3703 0.036 Uiso 1 1 calc R . .
H18B H -0.1650 0.5128 -0.4373 0.036 Uiso 1 1 calc R . .
H18C H -0.0729 0.5726 -0.3682 0.036 Uiso 1 1 calc R . .
O19 O 0.37741(12) 0.32987(11) -0.46741(7) 0.0228(3) Uani 1 1 d . . .
O20 O -0.06304(13) 0.20636(11) -0.44961(7) 0.0241(3) Uani 1 1 d . . .
C21 C -0.02834(16) 0.48108(14) -0.24299(9) 0.0181(3) Uani 1 1 d . . .
H21 H -0.0298 0.5511 -0.2573 0.022 Uiso 1 1 calc R . .
C22 C -0.05685(16) 0.39145(14) -0.29329(9) 0.0179(3) Uani 1 1 d . . .
C23 C -0.05605(18) 0.28698(14) -0.27062(9) 0.0214(4) Uani 1 1 d . . .
C24 C -0.02608(19) 0.27469(15) -0.20088(10) 0.0239(4) Uani 1 1 d . . .
H24 H -0.0267 0.2046 -0.1867 0.029 Uiso 1 1 calc R . .
C25 C 0.00482(18) 0.36617(15) -0.15210(9) 0.0212(4) Uani 1 1 d . . .
C26 C 0.00239(16) 0.47273(14) -0.17234(9) 0.0170(3) Uani 1 1 d . . .
C27 C 0.03306(16) 0.57408(14) -0.11953(9) 0.0173(3) Uani 1 1 d . . .
H27 H -0.0054 0.5559 -0.0815 0.021 Uiso 1 1 calc R . .
C28 C -0.03115(17) 0.67565(14) -0.14686(9) 0.0204(4) Uani 1 1 d . . .
H28A H -0.1252 0.6571 -0.1655 0.031 Uiso 1 1 calc R . .
H28B H 0.0085 0.6994 -0.1822 0.031 Uiso 1 1 calc R . .
H28C H -0.0167 0.7339 -0.1099 0.031 Uiso 1 1 calc R . .
O29 O -0.08475(15) 0.19113(10) -0.31485(7) 0.0296(3) Uani 1 1 d . . .
O30 O 0.03879(15) 0.34528(12) -0.08446(7) 0.0284(3) Uani 1 1 d . . .
C31 C 0.26538(17) 0.64463(14) -0.12760(9) 0.0178(3) Uani 1 1 d . . .
H31 H 0.2273 0.6550 -0.1731 0.021 Uiso 1 1 calc R . .
C32 C 0.18276(17) 0.60073(14) -0.08940(9) 0.0176(3) Uani 1 1 d . . .
C33 C 0.24360(17) 0.58167(14) -0.02228(9) 0.0183(3) Uani 1 1 d . . .
C34 C 0.38001(18) 0.60784(14) 0.00586(9) 0.0201(4) Uani 1 1 d . . .
H34 H 0.4186 0.5947 0.0508 0.024 Uiso 1 1 calc R . .
C35 C 0.45834(17) 0.65392(14) -0.03386(9) 0.0190(3) Uani 1 1 d . . .
C36 C 0.40193(17) 0.67388(14) -0.10144(9) 0.0176(3) Uani 1 1 d . . .
C37 C 0.48661(17) 0.72412(14) -0.14577(9) 0.0182(3) Uani 1 1 d . . .
H37 H 0.5745 0.7492 -0.1151 0.022 Uiso 1 1 calc R . .
C38 C 0.42920(18) 0.82543(14) -0.17605(9) 0.0225(4) Uani 1 1 d . . .
H38A H 0.4180 0.8772 -0.1396 0.034 Uiso 1 1 calc R . .
H38B H 0.3443 0.8037 -0.2080 0.034 Uiso 1 1 calc R . .
H38C H 0.4893 0.8590 -0.1996 0.034 Uiso 1 1 calc R . .
O39 O 0.16353(12) 0.53473(11) 0.01511(7) 0.0226(3) Uani 1 1 d . . .
O40 O 0.59411(12) 0.67784(11) -0.00866(7) 0.0223(3) Uani 1 1 d . . .
C41 C 0.74926(17) -0.12208(15) -0.27338(9) 0.0208(4) Uani 1 1 d . . .
C42 C 0.70762(17) -0.23218(15) -0.29748(9) 0.0217(4) Uani 1 1 d . . .
H42 H 0.6965 -0.2829 -0.2672 0.026 Uiso 1 1 calc R . .
C43 C 0.68319(17) -0.26468(15) -0.36731(9) 0.0211(4) Uani 1 1 d . . .
H43 H 0.6535 -0.3380 -0.3831 0.025 Uiso 1 1 calc R . .
N44 N 0.69999(15) -0.19633(12) -0.41357(7) 0.0210(3) Uani 1 1 d . . .
C45 C 0.74373(18) -0.09139(15) -0.38951(9) 0.0232(4) Uani 1 1 d . . .
H45 H 0.7588 -0.0435 -0.4207 0.028 Uiso 1 1 calc R . .
C46 C 0.76782(18) -0.05002(15) -0.32100(10) 0.0230(4) Uani 1 1 d . . .
H46 H 0.7957 0.0241 -0.3069 0.028 Uiso 1 1 calc R . .
C47 C 0.77048(19) -0.08490(16) -0.20130(10) 0.0253(4) Uani 1 1 d . . .
C48 C 0.78346(19) -0.05972(16) -0.14132(10) 0.0265(4) Uani 1 1 d . . .
C49 C 0.79945(18) -0.03421(16) -0.06842(9) 0.0246(4) Uani 1 1 d . . .
C50 C 0.7869(2) 0.07140(16) -0.03989(10) 0.0288(4) Uani 1 1 d . . .
H50 H 0.7679 0.1271 -0.0682 0.035 Uiso 1 1 calc R . .
C51 C 0.8026(2) 0.09345(16) 0.03040(10) 0.0283(4) Uani 1 1 d . . .
H51 H 0.7935 0.1638 0.0492 0.034 Uiso 1 1 calc R . .
C52 C 0.83197(18) 0.01031(16) 0.07325(9) 0.0240(4) Uani 1 1 d . . .
C53 C 0.84240(19) -0.09591(16) 0.04468(10) 0.0256(4) Uani 1 1 d . . .
H53 H 0.8608 -0.1517 0.0729 0.031 Uiso 1 1 calc R . .
C54 C 0.82523(19) -0.11780(16) -0.02571(10) 0.0260(4) Uani 1 1 d . . .
H54 H 0.8309 -0.1887 -0.0447 0.031 Uiso 1 1 calc R . .
C55 C 0.85398(19) 0.03299(16) 0.14677(10) 0.0259(4) Uani 1 1 d . . .
C56 C 0.87383(19) 0.04970(16) 0.20795(10) 0.0255(4) Uani 1 1 d . . .
C57 C 0.89248(17) 0.07109(15) 0.28089(9) 0.0222(4) Uani 1 1 d . . .
C58 C 0.92595(18) 0.17774(15) 0.31469(9) 0.0234(4) Uani 1 1 d . . .
H58 H 0.9375 0.2368 0.2901 0.028 Uiso 1 1 calc R . .
C59 C 0.94164(18) 0.19442(15) 0.38486(9) 0.0220(4) Uani 1 1 d . . .
H59 H 0.9656 0.2656 0.4068 0.026 Uiso 1 1 calc R . .
N60 N 0.92411(15) 0.11310(13) 0.42319(8) 0.0228(3) Uani 1 1 d . . .
C61 C 0.89271(19) 0.01121(15) 0.39057(10) 0.0261(4) Uani 1 1 d . . .
H61 H 0.8807 -0.0461 0.4164 0.031 Uiso 1 1 calc R . .
C62 C 0.87704(19) -0.01367(16) 0.32045(10) 0.0251(4) Uani 1 1 d . . .
H62 H 0.8565 -0.0860 0.3002 0.030 Uiso 1 1 calc R . .
C71 C 0.58588(19) 0.81178(16) 0.25846(10) 0.0253(4) Uani 1 1 d . . .
C72 C 0.5373(2) 0.86018(17) 0.19818(10) 0.0333(5) Uani 1 1 d . . .
H72 H 0.4896 0.9214 0.1991 0.040 Uiso 1 1 calc R . .
C73 C 0.5614(2) 0.81558(18) 0.13745(11) 0.0351(5) Uani 1 1 d . . .
H73 H 0.5289 0.8488 0.0978 0.042 Uiso 1 1 calc R . .
N74 N 0.62895(16) 0.72677(14) 0.13207(8) 0.0291(4) Uani 1 1 d . . .
C75 C 0.67542(19) 0.68139(16) 0.18987(10) 0.0271(4) Uani 1 1 d . . .
H75 H 0.7227 0.6202 0.1874 0.033 Uiso 1 1 calc R . .
C76 C 0.65713(19) 0.72054(16) 0.25356(10) 0.0259(4) Uani 1 1 d . . .
H76 H 0.6920 0.6863 0.2924 0.031 Uiso 1 1 calc R . .
C77 C 0.5644(2) 0.85786(16) 0.32311(10) 0.0270(4) Uani 1 1 d . . .
C78 C 0.5467(2) 0.89922(16) 0.37575(10) 0.0269(4) Uani 1 1 d . . .
C79 C 0.52400(19) 0.94980(16) 0.43901(10) 0.0250(4) Uani 1 1 d . . .
C80 C 0.58348(19) 1.05517(16) 0.46708(10) 0.0255(4) Uani 1 1 d . . .
H80 H 0.6396 1.0924 0.4451 0.031 Uiso 1 1 calc R . .
C81 C 0.4399(2) 0.89492(16) 0.47282(10) 0.0270(4) Uani 1 1 d . . .
H81 H 0.3995 0.8247 0.4549 0.032 Uiso 1 1 calc R . .
H20 H -0.063(2) 0.1677(19) -0.4904(13) 0.040(6) Uiso 1 1 d . . .
H9 H 0.653(2) 0.6123(19) -0.0862(12) 0.039(7) Uiso 1 1 d . . .
H10 H 0.521(2) 0.3827(19) -0.3805(13) 0.041(7) Uiso 1 1 d . . .
H39 H 0.210(2) 0.5153(19) 0.0503(12) 0.036(7) Uiso 1 1 d . . .
H40 H 0.611(2) 0.682(2) 0.0331(13) 0.044(7) Uiso 1 1 d . . .
H30 H 0.056(2) 0.405(2) -0.0565(12) 0.038(7) Uiso 1 1 d . . .
H29 H -0.087(3) 0.203(2) -0.3599(15) 0.067(9) Uiso 1 1 d . . .
H19 H 0.355(3) 0.274(2) -0.5049(15) 0.070(9) Uiso 1 1 d . . .

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(8) 0.0191(8) 0.0173(8) 0.0033(7) 0.0034(7) -0.0002(6)
C2 0.0148(8) 0.0187(8) 0.0168(8) 0.0027(6) 0.0057(6) -0.0022(6)
C3 0.0148(8) 0.0254(9) 0.0133(8) 0.0057(7) 0.0032(6) -0.0018(7)
C4 0.0159(8) 0.0213(9) 0.0234(9) 0.0050(7) 0.0044(7) 0.0025(7)
C5 0.0176(8) 0.0171(8) 0.0209(9) 0.0004(7) 0.0075(7) -0.0012(6)
C6 0.0164(8) 0.0166(8) 0.0172(8) 0.0021(6) 0.0035(7) -0.0031(6)
C7 0.0204(9) 0.0208(9) 0.0150(8) 0.0008(7) 0.0031(7) 0.0002(7)
C8 0.0236(9) 0.0244(9) 0.0179(9) 0.0038(7) 0.0003(7) -0.0016(7)
O9 0.0203(7) 0.0320(7) 0.0148(6) 0.0040(5) 0.0024(5) 0.0055(5)
O10 0.0224(7) 0.0266(7) 0.0233(7) -0.0058(6) 0.0017(6) 0.0047(5)
C11 0.0239(9) 0.0186(8) 0.0141(8) -0.0005(7) 0.0030(7) 0.0020(7)
C12 0.0193(9) 0.0201(9) 0.0136(8) 0.0028(6) -0.0002(7) -0.0014(7)
C13 0.0201(9) 0.0235(9) 0.0107(8) 0.0019(7) 0.0027(6) 0.0026(7)
C14 0.0268(9) 0.0195(9) 0.0138(8) -0.0011(7) 0.0034(7) -0.0001(7)
C15 0.0225(9) 0.0202(9) 0.0132(8) 0.0012(7) 0.0021(7) -0.0038(7)
C16 0.0204(9) 0.0210(9) 0.0136(8) 0.0013(7) 0.0029(7) -0.0003(7)
C17 0.0187(9) 0.0190(8) 0.0172(8) -0.0004(7) 0.0025(7) -0.0028(7)
C18 0.0231(9) 0.0259(10) 0.0205(9) 0.0035(7) 0.0011(7) 0.0028(7)
O19 0.0216(7) 0.0261(7) 0.0190(6) -0.0040(5) 0.0044(5) 0.0009(5)
O20 0.0284(7) 0.0239(7) 0.0175(6) -0.0054(5) 0.0070(5) -0.0087(5)
C21 0.0152(8) 0.0179(8) 0.0207(9) 0.0026(7) 0.0038(7) 0.0002(6)
C22 0.0148(8) 0.0195(8) 0.0191(9) 0.0016(7) 0.0045(7) -0.0009(6)
C23 0.0246(9) 0.0174(8) 0.0217(9) -0.0015(7) 0.0075(7) -0.0017(7)
C24 0.0319(10) 0.0173(9) 0.0244(10) 0.0055(7) 0.0098(8) 0.0010(7)
C25 0.0239(9) 0.0231(9) 0.0180(9) 0.0050(7) 0.0072(7) 0.0025(7)
C26 0.0131(8) 0.0191(8) 0.0186(8) 0.0004(7) 0.0045(6) 0.0005(6)
C27 0.0153(8) 0.0218(9) 0.0152(8) 0.0020(7) 0.0047(6) 0.0018(6)
C28 0.0184(9) 0.0213(9) 0.0208(9) 0.0001(7) 0.0042(7) 0.0024(7)
O29 0.0483(9) 0.0167(6) 0.0244(7) -0.0019(5) 0.0136(6) -0.0033(6)
O30 0.0469(9) 0.0231(7) 0.0160(7) 0.0042(6) 0.0081(6) 0.0059(6)
C31 0.0188(8) 0.0186(8) 0.0154(8) -0.0001(6) 0.0035(7) 0.0027(6)
C32 0.0163(8) 0.0182(8) 0.0172(8) -0.0009(6) 0.0031(7) 0.0010(6)
C33 0.0193(9) 0.0200(9) 0.0167(8) 0.0014(7) 0.0073(7) 0.0015(7)
C34 0.0221(9) 0.0258(9) 0.0118(8) 0.0016(7) 0.0036(7) 0.0024(7)
C35 0.0166(8) 0.0217(9) 0.0172(8) -0.0027(7) 0.0035(7) -0.0001(7)
C36 0.0192(8) 0.0177(8) 0.0157(8) -0.0011(6) 0.0054(7) 0.0005(6)
C37 0.0170(8) 0.0208(9) 0.0156(8) 0.0002(7) 0.0033(7) -0.0021(6)
C38 0.0258(10) 0.0195(9) 0.0224(9) 0.0008(7) 0.0078(7) -0.0005(7)
O39 0.0174(6) 0.0348(8) 0.0169(6) 0.0084(6) 0.0046(5) 0.0018(5)
O40 0.0163(6) 0.0353(8) 0.0131(6) -0.0008(5) 0.0015(5) -0.0016(5)
C41 0.0172(8) 0.0262(9) 0.0179(9) -0.0009(7) 0.0040(7) 0.0005(7)
C42 0.0204(9) 0.0248(9) 0.0201(9) 0.0049(7) 0.0053(7) -0.0002(7)
C43 0.0187(9) 0.0200(9) 0.0242(9) 0.0003(7) 0.0050(7) 0.0025(7)
N44 0.0203(8) 0.0248(8) 0.0171(7) 0.0000(6) 0.0033(6) 0.0048(6)
C45 0.0260(10) 0.0247(9) 0.0208(9) 0.0078(7) 0.0071(7) 0.0050(7)
C46 0.0243(9) 0.0195(9) 0.0241(9) 0.0013(7) 0.0046(7) 0.0014(7)
C47 0.0225(9) 0.0296(10) 0.0223(10) -0.0007(8) 0.0054(7) -0.0022(7)
C48 0.0232(10) 0.0320(10) 0.0224(10) -0.0013(8) 0.0049(8) -0.0010(8)
C49 0.0207(9) 0.0327(10) 0.0177(9) -0.0055(7) 0.0039(7) -0.0018(7)
C50 0.0338(11) 0.0288(10) 0.0217(10) 0.0004(8) 0.0044(8) 0.0018(8)
C51 0.0321(11) 0.0254(10) 0.0245(10) -0.0060(8) 0.0050(8) 0.0015(8)
C52 0.0211(9) 0.0305(10) 0.0178(9) -0.0053(7) 0.0039(7) -0.0004(7)
C53 0.0277(10) 0.0264(10) 0.0215(9) -0.0005(8) 0.0051(8) 0.0026(8)
C54 0.0285(10) 0.0263(10) 0.0222(9) -0.0057(8) 0.0079(8) 0.0015(8)
C55 0.0242(10) 0.0301(10) 0.0216(10) -0.0040(8) 0.0045(7) 0.0028(8)
C56 0.0231(9) 0.0278(10) 0.0237(10) -0.0033(8) 0.0047(8) 0.0021(8)
C57 0.0174(9) 0.0274(10) 0.0198(9) -0.0033(7) 0.0028(7) 0.0030(7)
C58 0.0255(10) 0.0242(9) 0.0194(9) 0.0025(7) 0.0039(7) 0.0008(7)
C59 0.0252(9) 0.0200(9) 0.0187(9) -0.0012(7) 0.0026(7) 0.0012(7)
N60 0.0236(8) 0.0250(8) 0.0180(8) 0.0004(6) 0.0034(6) 0.0003(6)
C61 0.0295(10) 0.0227(9) 0.0250(10) 0.0027(8) 0.0059(8) -0.0020(8)
C62 0.0247(10) 0.0221(9) 0.0249(10) -0.0041(7) 0.0028(8) -0.0016(7)
C71 0.0270(10) 0.0265(10) 0.0215(9) -0.0021(8) 0.0070(8) -0.0019(8)
C72 0.0431(13) 0.0306(11) 0.0270(11) 0.0022(9) 0.0085(9) 0.0104(9)
C73 0.0430(13) 0.0388(12) 0.0234(10) 0.0043(9) 0.0060(9) 0.0085(10)
N74 0.0276(9) 0.0362(10) 0.0219(8) -0.0027(7) 0.0060(7) 0.0001(7)
C75 0.0243(10) 0.0294(10) 0.0268(10) -0.0015(8) 0.0066(8) 0.0019(8)
C76 0.0263(10) 0.0271(10) 0.0232(10) 0.0014(8) 0.0053(8) -0.0003(8)
C77 0.0305(10) 0.0266(10) 0.0237(10) -0.0001(8) 0.0073(8) 0.0020(8)
C78 0.0290(10) 0.0274(10) 0.0243(10) 0.0020(8) 0.0065(8) 0.0052(8)
C79 0.0275(10) 0.0282(10) 0.0205(9) 0.0027(8) 0.0061(8) 0.0099(8)
C80 0.0265(10) 0.0271(10) 0.0255(10) 0.0057(8) 0.0095(8) 0.0062(8)
C81 0.0295(10) 0.0245(10) 0.0264(10) 0.0004(8) 0.0056(8) 0.0059(8)

_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 1.395(2) . ?
C1 C2 1.397(2) . ?
C2 C3 1.399(2) . ?
C2 C37 1.522(2) . ?
C3 C4 1.384(2) . ?
C3 O9 1.389(2) . ?
C4 C5 1.392(2) . ?
C5 O10 1.372(2) . ?
C5 C6 1.407(2) . ?
C6 C7 1.524(2) . ?
C7 C12 1.530(2) . ?
C7 C8 1.535(2) . ?
C11 C16 1.394(2) . ?
C11 C12 1.396(2) . ?
C12 C13 1.398(2) . ?
C13 O19 1.376(2) . ?
C13 C14 1.392(2) . ?
C14 C15 1.392(2) . ?
C15 O20 1.381(2) . ?
C15 C16 1.400(2) . ?
C16 C17 1.526(2) . ?
C17 C22 1.526(2) . ?
C17 C18 1.529(2) . ?
C21 C22 1.389(2) . ?
C21 C26 1.395(2) . ?
C22 C23 1.398(2) . ?
C23 O29 1.377(2) . ?
C23 C24 1.388(3) . ?
C24 C25 1.387(3) . ?
C25 O30 1.374(2) . ?
C25 C26 1.404(2) . ?
C26 C27 1.522(2) . ?
C27 C32 1.524(2) . ?
C27 C28 1.538(2) . ?
C31 C36 1.395(2) . ?
C31 C32 1.393(2) . ?
C32 C33 1.395(2) . ?
C33 O39 1.378(2) . ?
C33 C34 1.393(2) . ?
C34 C35 1.396(2) . ?
C35 O40 1.377(2) . ?
C35 C36 1.397(2) . ?
C36 C37 1.532(2) . ?
C37 C38 1.529(2) . ?
C41 C42 1.393(2) . ?
C41 C46 1.398(3) . ?
C41 C47 1.440(2) . ?
C42 C43 1.383(2) . ?
C43 N44 1.341(2) . ?
N44 C45 1.339(2) . ?
C45 C46 1.383(3) . ?
C47 C48 1.192(3) . ?
C48 C49 1.439(2) . ?
C49 C50 1.396(3) . ?
C49 C54 1.396(3) . ?
C50 C51 1.384(3) . ?
C51 C52 1.398(3) . ?
C52 C53 1.398(3) . ?
C52 C55 1.440(2) . ?
C53 C54 1.384(3) . ?
C55 C56 1.195(3) . ?
C56 C57 1.432(2) . ?
C57 C62 1.388(3) . ?
C57 C58 1.398(2) . ?
C58 C59 1.377(2) . ?
C59 N60 1.343(2) . ?
N60 C61 1.337(2) . ?
C61 C62 1.384(3) . ?
C71 C76 1.394(3) . ?
C71 C72 1.399(3) . ?
C71 C77 1.445(3) . ?
C72 C73 1.379(3) . ?
C73 N74 1.348(3) . ?
N74 C75 1.335(2) . ?
C75 C76 1.389(3) . ?
C77 C78 1.194(3) . ?
C78 C79 1.444(3) . ?
C79 C80 1.398(3) . ?
C79 C81 1.400(3) . ?
C80 C81 1.388(3) 2_676 ?
C81 C80 1.388(3) 2_676 ?

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 123.92(16) . . ?
C1 C2 C3 116.42(16) . . ?
C1 C2 C37 122.84(15) . . ?
C3 C2 C37 120.74(15) . . ?
C4 C3 O9 116.76(15) . . ?
C4 C3 C2 121.95(16) . . ?
O9 C3 C2 121.28(16) . . ?
C3 C4 C5 119.88(16) . . ?
O10 C5 C4 115.97(15) . . ?
O10 C5 C6 123.33(16) . . ?
C4 C5 C6 120.69(16) . . ?
C1 C6 C5 117.14(15) . . ?
C1 C6 C7 122.39(15) . . ?
C5 C6 C7 120.47(15) . . ?
C6 C7 C12 110.57(13) . . ?
C6 C7 C8 113.76(14) . . ?
C12 C7 C8 111.30(14) . . ?
C16 C11 C12 123.50(16) . . ?
C11 C12 C13 117.33(16) . . ?
C11 C12 C7 121.68(15) . . ?
C13 C12 C7 120.99(15) . . ?
O19 C13 C14 120.50(15) . . ?
O19 C13 C12 118.58(15) . . ?
C14 C13 C12 120.92(16) . . ?
C13 C14 C15 119.98(16) . . ?
O20 C15 C14 120.93(16) . . ?
O20 C15 C16 118.05(16) . . ?
C14 C15 C16 121.00(16) . . ?
C11 C16 C15 117.19(16) . . ?
C11 C16 C17 121.73(15) . . ?
C15 C16 C17 121.08(15) . . ?
C22 C17 C16 110.52(14) . . ?
C22 C17 C18 113.44(14) . . ?
C16 C17 C18 112.12(14) . . ?
C22 C21 C26 124.16(16) . . ?
C21 C22 C23 116.92(16) . . ?
C21 C22 C17 122.60(15) . . ?
C23 C22 C17 120.48(15) . . ?
O29 C23 C24 116.02(16) . . ?
O29 C23 C22 123.05(16) . . ?
C24 C23 C22 120.93(16) . . ?
C25 C24 C23 120.51(16) . . ?
O30 C25 C24 116.03(16) . . ?
O30 C25 C26 123.32(16) . . ?
C24 C25 C26 120.64(16) . . ?
C21 C26 C25 116.81(15) . . ?
C21 C26 C27 121.81(15) . . ?
C25 C26 C27 121.38(15) . . ?
C26 C27 C32 111.59(13) . . ?
C26 C27 C28 113.60(14) . . ?
C32 C27 C28 110.86(14) . . ?
C36 C31 C32 123.67(16) . . ?
C31 C32 C33 116.86(15) . . ?
C31 C32 C27 121.67(15) . . ?
C33 C32 C27 121.47(15) . . ?
O39 C33 C34 121.08(15) . . ?
O39 C33 C32 117.31(15) . . ?
C34 C33 C32 121.61(15) . . ?
C33 C34 C35 119.50(16) . . ?
O40 C35 C36 117.81(15) . . ?
O40 C35 C34 121.25(16) . . ?
C36 C35 C34 120.90(16) . . ?
C31 C36 C35 117.41(15) . . ?
C31 C36 C37 121.05(15) . . ?
C35 C36 C37 121.54(15) . . ?
C2 C37 C38 113.65(14) . . ?
C2 C37 C36 110.35(13) . . ?
C38 C37 C36 111.76(14) . . ?
C42 C41 C46 118.18(16) . . ?
C42 C41 C47 120.07(16) . . ?
C46 C41 C47 121.75(17) . . ?
C43 C42 C41 118.78(16) . . ?
N44 C43 C42 123.63(16) . . ?
C45 N44 C43 117.01(15) . . ?
N44 C45 C46 123.87(16) . . ?
C45 C46 C41 118.48(17) . . ?
C48 C47 C41 176.0(2) . . ?
C47 C48 C49 177.5(2) . . ?
C50 C49 C54 119.52(17) . . ?
C50 C49 C48 121.46(18) . . ?
C54 C49 C48 119.00(17) . . ?
C51 C50 C49 120.16(19) . . ?
C50 C51 C52 120.17(18) . . ?
C51 C52 C53 119.75(17) . . ?
C51 C52 C55 120.85(17) . . ?
C53 C52 C55 119.40(18) . . ?
C54 C53 C52 119.85(18) . . ?
C53 C54 C49 120.51(18) . . ?
C56 C55 C52 178.5(2) . . ?
C55 C56 C57 177.8(2) . . ?
C62 C57 C58 117.71(17) . . ?
C62 C57 C56 120.96(17) . . ?
C58 C57 C56 121.33(17) . . ?
C59 C58 C57 119.24(17) . . ?
N60 C59 C58 123.33(17) . . ?
C61 N60 C59 117.09(16) . . ?
N60 C61 C62 123.63(17) . . ?
C61 C62 C57 118.98(17) . . ?
C76 C71 C72 117.56(18) . . ?
C76 C71 C77 122.23(18) . . ?
C72 C71 C77 120.20(18) . . ?
C73 C72 C71 118.92(19) . . ?
N74 C73 C72 123.96(19) . . ?
C75 N74 C73 116.74(17) . . ?
N74 C75 C76 123.64(18) . . ?
C75 C76 C71 119.18(18) . . ?
C78 C77 C71 177.9(2) . . ?
C77 C78 C79 179.4(2) . . ?
C80 C79 C81 118.65(17) . . ?
C80 C79 C78 120.76(17) . . ?
C81 C79 C78 120.58(18) . . ?
C81 C80 C79 121.05(18) 2_676 . ?
C80 C81 C79 120.29(18) 2_676 . ?

_diffrn_measured_fraction_theta_max 0.912
_diffrn_reflns_theta_full        27.89
_diffrn_measured_fraction_theta_full 0.912
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.049

#===END

data_nakamura12
_database_code_CSD               214041

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42.75 H41.25 N2 O5.25'
_chemical_formula_weight         667.03

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)/m

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

_cell_length_a                   11.1453(5)
_cell_length_b                   24.7280(12)
_cell_length_c                   13.0970(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.4150(10)
_cell_angle_gamma                90.00
_cell_volume                     3525.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    116(2)
_cell_measurement_reflns_used    22365
_cell_measurement_theta_min      1.59
_cell_measurement_theta_max      27.90

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.22
_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             1415
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      116(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            22365
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         27.90
_reflns_number_total             8345
_reflns_number_gt                6926
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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^)+(0.1307P)^2^+5.0815P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8345
_refine_ls_number_parameters     567
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0774
_refine_ls_wR_factor_ref         0.2236
_refine_ls_wR_factor_gt          0.2096
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_restrained_S_all      0.917
_refine_ls_shift/su_max          0.153
_refine_ls_shift/su_mean         0.003

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 0.4485(3) 0.7500 0.8092(2) 0.0192(6) Uani 1 2 d S . .
H1 H 0.3774 0.7500 0.7568 0.023 Uiso 1 2 calc SR . .
C4 C 0.6606(6) 0.7500 0.9595(4) 0.077(2) Uani 1 2 d S . .
H4 H 0.7344 0.7500 1.0088 0.092 Uiso 1 2 calc SR . .
C5 C 0.6062(3) 0.70149(10) 0.9231(2) 0.0429(8) Uani 1 1 d . . .
C6 C 0.4992(2) 0.70040(8) 0.84656(16) 0.0185(4) Uani 1 1 d . . .
C7 C 0.4362(2) 0.64653(9) 0.81538(17) 0.0218(4) Uani 1 1 d . . .
H7 H 0.4990 0.6184 0.8344 0.026 Uiso 1 1 calc R . .
C8 C 0.3405(3) 0.63668(13) 0.8821(2) 0.0401(7) Uani 1 1 d . . .
H8A H 0.2998 0.6029 0.8626 0.060 Uiso 1 1 calc R . .
H8B H 0.2813 0.6654 0.8708 0.060 Uiso 1 1 calc R . .
H8C H 0.3808 0.6356 0.9546 0.060 Uiso 1 1 calc R . .
O10 O 0.6539(3) 0.65292(7) 0.96336(17) 0.0661(9) Uani 1 1 d . . .
H10 H 0.7216 0.6579 1.0017 0.099 Uiso 1 1 calc R . .
C11 C 0.25724(19) 0.64771(8) 0.65713(17) 0.0197(4) Uani 1 1 d . . .
H11 H 0.2079 0.6602 0.7011 0.024 Uiso 1 1 calc R . .
C12 C 0.3817(2) 0.64004(8) 0.69932(17) 0.0209(4) Uani 1 1 d . . .
C13 C 0.45426(19) 0.62189(8) 0.63158(18) 0.0215(4) Uani 1 1 d . . .
C14 C 0.40226(19) 0.61082(9) 0.52717(18) 0.0221(4) Uani 1 1 d . . .
H14 H 0.4514 0.5981 0.4832 0.027 Uiso 1 1 calc R . .
C15 C 0.27704(19) 0.61871(8) 0.48830(17) 0.0200(4) Uani 1 1 d . . .
C16 C 0.20217(19) 0.63784(8) 0.55300(17) 0.0197(4) Uani 1 1 d . . .
C17 C 0.06597(18) 0.64762(9) 0.50851(17) 0.0197(4) Uani 1 1 d . . .
H17 H 0.0369 0.6183 0.4590 0.024 Uiso 1 1 calc R . .
C18 C -0.0116(2) 0.64602(10) 0.59218(18) 0.0244(5) Uani 1 1 d . . .
H18A H -0.0963 0.6523 0.5600 0.037 Uiso 1 1 calc R . .
H18B H 0.0164 0.6735 0.6435 0.037 Uiso 1 1 calc R . .
H18C H -0.0034 0.6112 0.6254 0.037 Uiso 1 1 calc R . .
O19 O 0.57704(14) 0.61404(7) 0.67112(13) 0.0267(4) Uani 1 1 d . . .
H19 H 0.6090 0.6016 0.6254 0.040 Uiso 1 1 calc R . .
O20 O 0.22414(14) 0.60688(7) 0.38595(12) 0.0248(4) Uani 1 1 d . . .
H20 H 0.2771 0.5960 0.3561 0.037 Uiso 1 1 calc R . .
C21 C 0.0621(3) 0.7500 0.4980(2) 0.0203(6) Uani 1 2 d S . .
H21 H 0.0822 0.7500 0.5707 0.024 Uiso 1 2 calc SR . .
C22 C 0.04807(18) 0.70038(8) 0.44714(17) 0.0199(4) Uani 1 1 d . . .
C23 C 0.02165(19) 0.70143(8) 0.33781(17) 0.0205(4) Uani 1 1 d . . .
C24 C 0.0072(3) 0.7500 0.2837(3) 0.0232(6) Uani 1 2 d S . .
H24 H -0.0121 0.7500 0.2110 0.028 Uiso 1 2 calc SR . .
O29 O 0.00985(15) 0.65461(6) 0.27863(13) 0.0255(4) Uani 1 1 d . . .
H29 H 0.0626 0.6328 0.3058 0.038 Uiso 1 1 calc R . .
C31 C 0.5552(2) 0.54386(9) 0.15345(16) 0.0221(4) Uani 1 1 d . . .
C32 C 0.5259(2) 0.50687(9) 0.22497(19) 0.0276(5) Uani 1 1 d . . .
H32 H 0.5593 0.4723 0.2310 0.033 Uiso 1 1 calc R . .
C33 C 0.4462(2) 0.52298(10) 0.2864(2) 0.0296(5) Uani 1 1 d . . .
H33 H 0.4270 0.4982 0.3338 0.036 Uiso 1 1 calc R . .
N34 N 0.39476(18) 0.57191(8) 0.28209(16) 0.0274(4) Uani 1 1 d . . .
C35 C 0.4260(2) 0.60743(10) 0.21522(19) 0.0297(5) Uani 1 1 d . . .
H35 H 0.3922 0.6419 0.2120 0.036 Uiso 1 1 calc R . .
C36 C 0.5056(2) 0.59564(10) 0.15074(17) 0.0275(5) Uani 1 1 d . . .
H36 H 0.5258 0.6218 0.1063 0.033 Uiso 1 1 calc R . .
C37 C 0.6343(2) 0.53000(10) 0.08473(18) 0.0258(5) Uani 1 1 d . . .
C38 C 0.6984(2) 0.52055(10) 0.02493(18) 0.0288(5) Uani 1 1 d . . .
C39 C 0.7762(2) 0.51055(11) -0.04745(18) 0.0303(5) Uani 1 1 d . . .
C40 C 0.8466(3) 0.46334(12) -0.0393(2) 0.0388(6) Uani 1 1 d . . .
H40 H 0.8409 0.4378 0.0115 0.047 Uiso 1 1 calc R . .
C41 C 0.9252(3) 0.45445(13) -0.1068(2) 0.0425(7) Uani 1 1 d . . .
H41 H 0.9726 0.4232 -0.1008 0.051 Uiso 1 1 calc R . .
C42 C 0.9330(2) 0.49270(12) -0.18405(19) 0.0336(6) Uani 1 1 d . . .
C43 C 0.8619(2) 0.53882(13) -0.1925(2) 0.0386(6) Uani 1 1 d . . .
H43 H 0.8662 0.5641 -0.2441 0.046 Uiso 1 1 calc R . .
C44 C 0.7839(2) 0.54778(13) -0.1246(2) 0.0371(6) Uani 1 1 d . . .
H44 H 0.7365 0.5791 -0.1310 0.045 Uiso 1 1 calc R . .
C45 C 1.0149(2) 0.48281(12) -0.25312(19) 0.0342(6) Uani 1 1 d . . .
C46 C 1.0835(2) 0.47245(11) -0.30846(18) 0.0292(5) Uani 1 1 d . . .
C47 C 1.16219(19) 0.45838(10) -0.37737(18) 0.0239(5) Uani 1 1 d . . .
C48 C 1.1710(2) 0.49090(9) -0.46198(18) 0.0237(5) Uani 1 1 d . . .
H48 H 1.1281 0.5234 -0.4734 0.028 Uiso 1 1 calc R . .
C49 C 1.2441(2) 0.47448(10) -0.52884(18) 0.0250(5) Uani 1 1 d . . .
H49 H 1.2481 0.4964 -0.5857 0.030 Uiso 1 1 calc R . .
N50 N 1.30942(17) 0.42873(8) -0.51642(16) 0.0254(4) Uani 1 1 d . . .
C51 C 1.3023(2) 0.39760(10) -0.43397(19) 0.0273(5) Uani 1 1 d . . .
H51 H 1.3479 0.3658 -0.4237 0.033 Uiso 1 1 calc R . .
C52 C 1.2305(2) 0.41051(10) -0.36354(18) 0.0263(5) Uani 1 1 d . . .
H52 H 1.2277 0.3877 -0.3077 0.032 Uiso 1 1 calc R . .
C61 C 0.3947(7) 0.7500 0.3149(5) 0.0251(14) Uani 0.50 2 d SPD A 1
C62 C 0.5231(12) 0.7500 0.3134(8) 0.028(3) Uani 0.50 2 d SPD A 1
H62 H 0.5819 0.7500 0.3756 0.033 Uiso 0.50 2 calc SPR A 1
C63 C 0.5582(6) 0.7500 0.2188(6) 0.0307(15) Uani 0.50 2 d SPD A 1
C64 C 0.4724(6) 0.7500 0.1254(6) 0.0325(15) Uani 0.50 2 d SPD A 1
H64 H 0.4984 0.7500 0.0625 0.039 Uiso 0.50 2 calc SPR A 1
C65 C 0.3486(6) 0.7500 0.1248(6) 0.0306(14) Uani 0.50 2 d SPD A 1
H65 H 0.2913 0.7500 0.0616 0.037 Uiso 0.50 2 calc SPR A 1
C66 C 0.3093(6) 0.7500 0.2196(6) 0.0275(14) Uani 0.50 2 d SPD A 1
H66 H 0.2257 0.7500 0.2190 0.033 Uiso 0.50 2 calc SPR A 1
C67 C 0.3531(8) 0.7500 0.4175(7) 0.0313(16) Uani 0.50 2 d SPD A 1
H67A H 0.2702 0.7630 0.4063 0.047 Uiso 0.25 1 calc PR A 1
H67B H 0.4059 0.7731 0.4665 0.047 Uiso 0.25 1 calc PR A 1
H67C H 0.3570 0.7139 0.4448 0.047 Uiso 0.25 1 calc PR A 1
C68 C 0.6928(7) 0.7500 0.2221(7) 0.054(3) Uani 0.50 2 d SPD A 1
H68A H 0.7373 0.7487 0.2935 0.081 Uiso 0.50 2 calc SPR A 1
H68B H 0.7144 0.7823 0.1896 0.081 Uiso 0.25 1 calc PR A 1
H68C H 0.7135 0.7190 0.1853 0.081 Uiso 0.25 1 calc PR A 1
O101 O 0.691(2) 0.7500 0.6089(12) 0.170(8) Uani 0.50 2 d SPD B 1
H101 H 0.7416 0.7531 0.5722 0.254 Uiso 0.25 1 calc PR B 1
C102 C 0.7534(11) 0.7500 0.7178(8) 0.080(5) Uani 0.50 2 d SPD B 1
H10A H 0.8293 0.7296 0.7273 0.096 Uiso 0.25 1 calc PR B 1
H10B H 0.7018 0.7337 0.7603 0.096 Uiso 0.25 1 calc PR B 1
C103 C 0.7805(9) 0.8099(4) 0.7498(9) 0.101(4) Uani 0.50 1 d PD B 1
H10C H 0.8214 0.8117 0.8222 0.152 Uiso 0.50 1 calc PR B 1
H10D H 0.7047 0.8297 0.7395 0.152 Uiso 0.50 1 calc PR B 1
H10E H 0.8322 0.8255 0.7077 0.152 Uiso 0.50 1 calc PR B 1
C71 C 0.4717(6) 0.7500 0.3846(7) 0.0365(17) Uani 0.50 2 d SPD C 2
C72 C 0.5279(7) 0.7500 0.4919(7) 0.0398(18) Uani 0.50 2 d SPD C 2
H72 H 0.4799 0.7500 0.5419 0.048 Uiso 0.50 2 calc SPR C 2
C73 C 0.6528(7) 0.7500 0.5222(7) 0.0376(17) Uani 0.50 2 d SPD C 2
C74 C 0.7266(7) 0.7500 0.4504(7) 0.0408(19) Uani 0.50 2 d SPD C 2
H74 H 0.8117 0.7500 0.4725 0.049 Uiso 0.50 2 calc SPR C 2
C75 C 0.6729(7) 0.7500 0.3454(7) 0.0411(19) Uani 0.50 2 d SPD C 2
H75 H 0.7227 0.7500 0.2968 0.049 Uiso 0.50 2 calc SPR C 2
C76 C 0.5449(14) 0.7500 0.3100(14) 0.062(6) Uani 0.50 2 d SPD C 2
H76 H 0.5096 0.7500 0.2388 0.074 Uiso 0.50 2 calc SPR C 2
C77 C 0.3351(8) 0.7500 0.3514(11) 0.051(2) Uani 0.50 2 d SPD C 2
H77A H 0.3008 0.7295 0.4004 0.077 Uiso 0.25 1 calc PR C 2
H77B H 0.3112 0.7340 0.2832 0.077 Uiso 0.25 1 calc PR C 2
H77C H 0.3054 0.7865 0.3490 0.077 Uiso 0.25 1 calc PR C 2
C78 C 0.7061(11) 0.7500 0.6329(11) 0.058(4) Uani 0.50 2 d SPD C 2
H78A H 0.6957 0.7150 0.6615 0.088 Uiso 0.25 1 calc PR C 2
H78B H 0.6658 0.7767 0.6669 0.088 Uiso 0.25 1 calc PR C 2
H78C H 0.7921 0.7583 0.6440 0.088 Uiso 0.25 1 calc PR C 2
O81 O 0.1391(6) 0.1616(3) -0.0877(5) 0.0588(14) Uani 0.50 1 d PD D 1
H81 H 0.1065 0.1532 -0.1479 0.088 Uiso 0.50 1 calc PR D 1
C82 C 0.0472(14) 0.1834(5) -0.0358(8) 0.226(19) Uani 0.50 1 d PD D 1
H82A H -0.0311 0.1700 -0.0748 0.271 Uiso 0.50 1 calc PR D 1
H82B H 0.0467 0.2221 -0.0479 0.271 Uiso 0.50 1 calc PR D 1
C83 C 0.0437(8) 0.1765(5) 0.0803(7) 0.088(4) Uani 0.50 1 d PD D 1
H83A H -0.0274 0.1945 0.0942 0.133 Uiso 0.50 1 calc PR D 1
H83B H 0.1165 0.1919 0.1230 0.133 Uiso 0.50 1 calc PR D 1
H83C H 0.0397 0.1387 0.0960 0.133 Uiso 0.50 1 calc PR D 1
O91 O 0.0837(4) 0.3363(2) -0.0555(4) 0.0360(12) Uani 0.50 1 d PD E 2
H91 H 0.0543 0.3375 -0.1185 0.054 Uiso 0.50 1 calc PR E 2
C92 C -0.0133(9) 0.3324(5) 0.0002(9) 0.102(5) Uani 0.50 1 d PD E 2
H92A H -0.0674 0.3032 -0.0307 0.123 Uiso 0.50 1 calc PR E 2
H92B H -0.0606 0.3656 -0.0114 0.123 Uiso 0.50 1 calc PR E 2
C93 C 0.0217(18) 0.3227(5) 0.1163(8) 0.148(9) Uani 0.50 1 d PD E 2
H93A H -0.0512 0.3206 0.1440 0.222 Uiso 0.50 1 calc PR E 2
H93B H 0.0722 0.3520 0.1491 0.222 Uiso 0.50 1 calc PR E 2
H93C H 0.0666 0.2894 0.1297 0.222 Uiso 0.50 1 calc PR E 2

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 0.0168(13) 0.0204(14) 0.0222(14) 0.000 0.0082(11) 0.000
C4 0.111(4) 0.0229(19) 0.058(3) 0.000 -0.067(3) 0.000
C5 0.072(2) 0.0183(12) 0.0238(12) 0.0025(9) -0.0215(12) 0.0029(12)
C6 0.0250(10) 0.0162(9) 0.0156(9) -0.0021(7) 0.0070(8) -0.0020(8)
C7 0.0213(10) 0.0164(10) 0.0271(11) 0.0028(8) 0.0037(8) -0.0008(8)
C8 0.0329(14) 0.0556(18) 0.0314(13) 0.0200(12) 0.0058(10) -0.0101(12)
O10 0.108(2) 0.0158(9) 0.0451(12) 0.0016(8) -0.0501(13) 0.0029(10)
C11 0.0189(10) 0.0135(9) 0.0277(11) -0.0016(8) 0.0075(8) -0.0007(7)
C12 0.0209(10) 0.0135(9) 0.0281(11) 0.0002(8) 0.0047(8) -0.0014(8)
C13 0.0167(10) 0.0161(9) 0.0313(11) 0.0029(8) 0.0047(8) -0.0002(7)
C14 0.0169(10) 0.0218(10) 0.0295(11) 0.0011(9) 0.0091(8) 0.0011(8)
C15 0.0178(10) 0.0176(9) 0.0248(10) 0.0000(8) 0.0050(8) -0.0019(8)
C16 0.0169(10) 0.0150(9) 0.0278(11) 0.0016(8) 0.0062(8) -0.0013(7)
C17 0.0157(10) 0.0191(10) 0.0253(10) -0.0012(8) 0.0065(8) -0.0012(8)
C18 0.0178(10) 0.0265(11) 0.0301(11) 0.0048(9) 0.0076(8) -0.0034(8)
O19 0.0150(7) 0.0306(9) 0.0345(9) 0.0001(7) 0.0054(6) 0.0035(6)
O20 0.0186(7) 0.0298(8) 0.0267(8) -0.0043(7) 0.0065(6) 0.0023(6)
C21 0.0153(13) 0.0227(15) 0.0249(15) 0.000 0.0087(11) 0.000
C22 0.0129(9) 0.0192(10) 0.0285(11) 0.0016(8) 0.0064(8) -0.0003(7)
C23 0.0147(9) 0.0200(10) 0.0265(11) -0.0027(8) 0.0038(8) -0.0016(8)
C24 0.0166(14) 0.0262(15) 0.0264(15) 0.000 0.0038(12) 0.000
O29 0.0274(8) 0.0191(8) 0.0272(8) -0.0023(6) -0.0002(6) 0.0009(6)
C31 0.0189(10) 0.0286(11) 0.0184(10) -0.0035(8) 0.0033(8) -0.0026(8)
C32 0.0309(12) 0.0208(11) 0.0357(13) -0.0025(9) 0.0177(10) -0.0017(9)
C33 0.0326(13) 0.0254(12) 0.0354(13) -0.0022(10) 0.0176(10) -0.0049(10)
N34 0.0228(9) 0.0334(11) 0.0267(10) -0.0082(8) 0.0070(8) -0.0008(8)
C35 0.0303(12) 0.0306(12) 0.0260(11) -0.0014(9) 0.0015(9) 0.0103(10)
C36 0.0344(13) 0.0293(12) 0.0174(10) 0.0039(9) 0.0025(9) 0.0028(10)
C37 0.0257(11) 0.0308(12) 0.0213(10) 0.0004(9) 0.0056(9) -0.0016(9)
C38 0.0254(12) 0.0378(13) 0.0242(11) -0.0014(10) 0.0078(9) -0.0035(10)
C39 0.0221(11) 0.0484(15) 0.0214(11) -0.0034(10) 0.0074(9) -0.0052(10)
C40 0.0464(16) 0.0400(15) 0.0377(14) 0.0010(12) 0.0263(12) -0.0025(12)
C41 0.0446(16) 0.0446(16) 0.0464(16) -0.0037(13) 0.0278(13) -0.0007(13)
C42 0.0242(12) 0.0541(16) 0.0245(12) -0.0066(11) 0.0099(9) -0.0072(11)
C43 0.0317(13) 0.0614(18) 0.0244(12) 0.0106(12) 0.0101(10) -0.0003(12)
C44 0.0286(13) 0.0566(17) 0.0271(12) 0.0077(12) 0.0082(10) 0.0070(12)
C45 0.0269(12) 0.0516(16) 0.0259(12) -0.0046(11) 0.0096(10) -0.0103(11)
C46 0.0249(12) 0.0402(14) 0.0232(11) -0.0017(10) 0.0068(9) -0.0077(10)
C47 0.0164(10) 0.0323(12) 0.0237(10) -0.0017(9) 0.0054(8) -0.0057(9)
C48 0.0202(10) 0.0247(11) 0.0276(11) 0.0011(9) 0.0086(8) 0.0010(8)
C49 0.0224(11) 0.0293(12) 0.0251(11) 0.0031(9) 0.0090(9) -0.0022(9)
N50 0.0170(9) 0.0295(10) 0.0307(10) -0.0013(8) 0.0074(7) -0.0004(7)
C51 0.0177(10) 0.0266(11) 0.0357(12) 0.0035(10) 0.0016(9) -0.0008(9)
C52 0.0176(10) 0.0337(12) 0.0259(11) 0.0075(9) 0.0005(8) -0.0061(9)
C61 0.028(4) 0.015(3) 0.039(4) 0.000 0.020(3) 0.000
C62 0.033(5) 0.037(7) 0.015(4) 0.000 0.009(3) 0.000
C63 0.027(3) 0.042(4) 0.028(4) 0.000 0.015(3) 0.000
C64 0.030(4) 0.034(4) 0.036(4) 0.000 0.013(3) 0.000
C65 0.029(3) 0.026(3) 0.034(4) 0.000 0.001(3) 0.000
C66 0.014(3) 0.030(3) 0.042(4) 0.000 0.013(3) 0.000
C67 0.037(4) 0.030(4) 0.030(4) 0.000 0.017(4) 0.000
C68 0.027(4) 0.103(8) 0.033(4) 0.000 0.009(3) 0.000
O101 0.17(2) 0.18(2) 0.154(18) 0.000 0.025(15) 0.000
C102 0.052(6) 0.155(15) 0.030(5) 0.000 0.005(4) 0.000
C103 0.064(6) 0.149(10) 0.092(7) -0.055(7) 0.020(5) -0.008(6)
C71 0.024(4) 0.021(3) 0.065(6) 0.000 0.010(4) 0.000
C72 0.037(4) 0.024(3) 0.065(5) 0.000 0.025(4) 0.000
C73 0.031(4) 0.025(3) 0.056(5) 0.000 0.007(4) 0.000
C74 0.025(4) 0.028(4) 0.074(6) 0.000 0.019(4) 0.000
C75 0.035(4) 0.035(4) 0.060(5) 0.000 0.025(4) 0.000
C76 0.056(9) 0.028(7) 0.102(15) 0.000 0.016(8) 0.000
C77 0.026(5) 0.042(5) 0.086(9) 0.000 0.010(6) 0.000
C78 0.048(6) 0.011(3) 0.130(13) 0.000 0.048(7) 0.000
O81 0.056(4) 0.058(3) 0.048(3) -0.008(3) -0.022(3) 0.003(3)
C82 0.42(4) 0.044(7) 0.110(14) 0.016(8) -0.17(2) -0.027(14)
C83 0.066(5) 0.113(9) 0.063(6) -0.033(6) -0.038(5) 0.042(6)
O91 0.030(2) 0.051(3) 0.025(2) -0.007(2) 0.0007(17) 0.009(2)
C92 0.071(6) 0.143(12) 0.110(9) 0.076(9) 0.057(7) 0.040(7)
C93 0.34(2) 0.054(6) 0.082(8) -0.014(6) 0.126(12) 0.010(9)

_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 1.395(2) 4_575 ?
C1 C6 1.395(2) . ?
C4 C5 1.382(3) . ?
C4 C5 1.382(3) 4_575 ?
C5 O10 1.372(3) . ?
C5 C6 1.383(3) . ?
C6 C7 1.520(3) . ?
C7 C12 1.519(3) . ?
C7 C8 1.536(3) . ?
C11 C12 1.391(3) . ?
C11 C16 1.392(3) . ?
C12 C13 1.397(3) . ?
C13 O19 1.369(3) . ?
C13 C14 1.393(3) . ?
C14 C15 1.393(3) . ?
C15 O20 1.375(3) . ?
C15 C16 1.394(3) . ?
C16 C17 1.524(3) . ?
C17 C22 1.523(3) . ?
C17 C18 1.535(3) . ?
C21 C22 1.389(3) 4_575 ?
C21 C22 1.389(3) . ?
C22 C23 1.399(3) . ?
C23 O29 1.384(3) . ?
C23 C24 1.386(3) . ?
C24 C23 1.386(3) 4_575 ?
C31 C36 1.392(3) . ?
C31 C32 1.397(3) . ?
C31 C37 1.431(3) . ?
C32 C33 1.379(3) . ?
C33 N34 1.335(3) . ?
N34 C35 1.338(3) . ?
C35 C36 1.382(3) . ?
C37 C38 1.191(3) . ?
C38 C39 1.438(3) . ?
C39 C44 1.383(4) . ?
C39 C40 1.398(4) . ?
C40 C41 1.389(3) . ?
C41 C42 1.401(4) . ?
C42 C43 1.379(4) . ?
C42 C45 1.438(3) . ?
C43 C44 1.389(4) . ?
C45 C46 1.189(3) . ?
C46 C47 1.430(3) . ?
C47 C48 1.390(3) . ?
C47 C52 1.398(3) . ?
C48 C49 1.379(3) . ?
C49 N50 1.336(3) . ?
N50 C51 1.342(3) . ?
C51 C52 1.382(3) . ?
C61 C66 1.398(10) . ?
C61 C62 1.435(14) . ?
C61 C67 1.512(8) . ?
C62 C63 1.378(11) . ?
C63 C64 1.381(10) . ?
C63 C68 1.492(10) . ?
C64 C65 1.378(9) . ?
C65 C66 1.403(9) . ?
O101 C102 1.446(10) . ?
C102 C103 1.552(8) . ?
C71 C76 1.402(15) . ?
C71 C72 1.411(12) . ?
C71 C77 1.490(10) . ?
C72 C73 1.364(10) . ?
C73 C74 1.376(10) . ?
C73 C78 1.444(14) . ?
C74 C75 1.376(11) . ?
C75 C76 1.402(16) . ?
O81 C82 1.450(9) . ?
C82 C83 1.538(9) . ?
O91 C92 1.431(8) . ?
C92 C93 1.505(9) . ?

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 C6 123.2(3) 4_575 . ?
C5 C4 C5 120.5(4) . 4_575 ?
O10 C5 C4 121.5(3) . . ?
O10 C5 C6 117.7(2) . . ?
C4 C5 C6 120.9(2) . . ?
C5 C6 C1 117.3(2) . . ?
C5 C6 C7 119.23(19) . . ?
C1 C6 C7 123.2(2) . . ?
C12 C7 C6 115.05(17) . . ?
C12 C7 C8 112.07(19) . . ?
C6 C7 C8 108.9(2) . . ?
C12 C11 C16 123.9(2) . . ?
C11 C12 C13 117.1(2) . . ?
C11 C12 C7 122.19(19) . . ?
C13 C12 C7 120.54(19) . . ?
O19 C13 C14 121.0(2) . . ?
O19 C13 C12 118.3(2) . . ?
C14 C13 C12 120.74(19) . . ?
C15 C14 C13 120.3(2) . . ?
O20 C15 C14 120.84(19) . . ?
O20 C15 C16 118.54(18) . . ?
C14 C15 C16 120.6(2) . . ?
C11 C16 C15 117.38(19) . . ?
C11 C16 C17 122.69(19) . . ?
C15 C16 C17 119.93(19) . . ?
C22 C17 C16 110.15(16) . . ?
C22 C17 C18 111.65(17) . . ?
C16 C17 C18 112.99(18) . . ?
C22 C21 C22 124.2(3) 4_575 . ?
C21 C22 C23 116.8(2) . . ?
C21 C22 C17 121.0(2) . . ?
C23 C22 C17 122.09(19) . . ?
O29 C23 C24 116.9(2) . . ?
O29 C23 C22 122.11(19) . . ?
C24 C23 C22 121.0(2) . . ?
C23 C24 C23 120.1(3) 4_575 . ?
C36 C31 C32 118.1(2) . . ?
C36 C31 C37 119.9(2) . . ?
C32 C31 C37 122.0(2) . . ?
C33 C32 C31 118.3(2) . . ?
N34 C33 C32 124.2(2) . . ?
C33 N34 C35 116.9(2) . . ?
N34 C35 C36 123.6(2) . . ?
C35 C36 C31 118.8(2) . . ?
C38 C37 C31 177.0(3) . . ?
C37 C38 C39 178.6(3) . . ?
C44 C39 C40 119.3(2) . . ?
C44 C39 C38 120.5(3) . . ?
C40 C39 C38 120.1(2) . . ?
C41 C40 C39 120.3(3) . . ?
C40 C41 C42 119.8(3) . . ?
C43 C42 C41 119.5(2) . . ?
C43 C42 C45 121.4(2) . . ?
C41 C42 C45 119.0(3) . . ?
C42 C43 C44 120.5(2) . . ?
C39 C44 C43 120.5(3) . . ?
C46 C45 C42 177.2(3) . . ?
C45 C46 C47 177.5(3) . . ?
C48 C47 C52 117.6(2) . . ?
C48 C47 C46 121.4(2) . . ?
C52 C47 C46 121.0(2) . . ?
C49 C48 C47 119.2(2) . . ?
N50 C49 C48 123.6(2) . . ?
C49 N50 C51 117.3(2) . . ?
N50 C51 C52 123.2(2) . . ?
C51 C52 C47 119.1(2) . . ?
C66 C61 C62 118.5(7) . . ?
C66 C61 C67 120.9(7) . . ?
C62 C61 C67 120.6(7) . . ?
C63 C62 C61 119.3(9) . . ?
C62 C63 C64 121.3(8) . . ?
C62 C63 C68 116.9(8) . . ?
C64 C63 C68 121.8(6) . . ?
C65 C64 C63 120.5(6) . . ?
C64 C65 C66 119.8(6) . . ?
C61 C66 C65 120.5(6) . . ?
O101 C102 C103 106.9(6) . . ?
C76 C71 C72 119.6(9) . . ?
C76 C71 C77 120.5(11) . . ?
C72 C71 C77 119.9(9) . . ?
C73 C72 C71 119.8(7) . . ?
C72 C73 C74 121.6(8) . . ?
C72 C73 C78 117.7(8) . . ?
C74 C73 C78 120.6(8) . . ?
C73 C74 C75 119.1(7) . . ?
C74 C75 C76 121.6(10) . . ?
C75 C76 C71 118.2(13) . . ?
O81 C82 C83 126.3(10) . . ?
O91 C92 C93 117.7(9) . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        27.90
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.070

#===END