 
data_1corr 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C35 H34 Bi N3 O7' 
_chemical_formula_weight          817.63 
 
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' 
 'Bi'  'Bi'  -4.1077  10.2566 
 '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                    11.221(2) 
_cell_length_b                    11.789(2) 
_cell_length_c                    14.441(3) 
_cell_angle_alpha                 66.93(3) 
_cell_angle_beta                  89.68(3) 
_cell_angle_gamma                 69.93(3) 
_cell_volume                      1632.2(6) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     5844 
_cell_measurement_theta_min       4.462 
_cell_measurement_theta_max       53.286 
 
_exptl_crystal_description        'plate' 
_exptl_crystal_colour             'colorless' 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.16 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.664 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              808 
_exptl_absorpt_coefficient_mu     5.454 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.289
_exptl_absorpt_correction_T_max   0.652
_exptl_absorpt_process_details    'SADABS (Scheldrick, 1996)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       298(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             16303 
_diffrn_reflns_av_R_equivalents   0.1491 
_diffrn_reflns_av_sigmaI/netI     0.3243 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          1.95 
_diffrn_reflns_theta_max          28.37 
_reflns_number_total              6803 
_reflns_number_gt                 2836 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'SHELXTL 6.10 (Bruker AXS, 2001)' 
_computing_cell_refinement        'SHELXTL 6.10 (Bruker AXS, 2001)' 
_computing_data_reduction         'SHELXTL 6.10 (Bruker AXS, 2001)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL 6.10 (Bruker AXS, 2001)' 
_computing_publication_material   'SHELXTL 6.10 (Bruker AXS, 2001)' 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0468P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          6803 
_refine_ls_number_parameters      373 
_refine_ls_number_restraints      6 
_refine_ls_R_factor_all           0.2033 
_refine_ls_R_factor_gt            0.0679 
_refine_ls_wR_factor_ref          0.1636 
_refine_ls_wR_factor_gt           0.1238 
_refine_ls_goodness_of_fit_ref    0.869 
_refine_ls_restrained_S_all       0.868 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Bi1 Bi -0.30835(6) 0.83542(6) 0.10060(4) 0.03915(19) Uani 1 1 d . . . 
O21 O -0.4747(9) 1.0225(9) 0.1198(8) 0.057(3) Uani 1 1 d . . . 
O22 O -0.4811(9) 0.8261(10) 0.2206(8) 0.056(3) Uani 1 1 d D . . 
O23 O -0.6594(10) 0.8106(11) 0.3325(8) 0.070(3) Uani 1 1 d D . . 
H23B H -0.5924(14) 0.775(3) 0.3095(12) 0.084 Uiso 1 1 d D . . 
O32 O -0.2493(10) 0.6025(8) 0.1988(7) 0.055(3) Uani 1 1 d D . . 
O31 O -0.3388(14) 0.6088(13) 0.0606(9) 0.088(4) Uani 1 1 d . . . 
O33 O -0.2456(16) 0.4244(16) 0.3726(12) 0.123(5) Uani 1 1 d D . . 
H33B H -0.227(2) 0.4917(18) 0.3362(13) 0.148 Uiso 1 1 d D . . 
C11 C -0.1844(8) 0.8229(10) 0.2289(6) 0.055(4) Uani 1 1 d G . . 
C12 C -0.2094(8) 0.9340(8) 0.2494(7) 0.048(4) Uani 1 1 d G . . 
H12A H -0.2766 1.0128 0.2100 0.058 Uiso 1 1 calc R . . 
C13 C -0.1341(11) 0.9273(10) 0.3289(8) 0.070(5) Uani 1 1 d G . . 
H13A H -0.1509 1.0016 0.3427 0.084 Uiso 1 1 calc R . . 
C14 C -0.0337(10) 0.8095(13) 0.3878(7) 0.073(5) Uani 1 1 d G . . 
H14A H 0.0168 0.8050 0.4410 0.088 Uiso 1 1 calc R . . 
C15 C -0.0086(9) 0.6985(10) 0.3673(8) 0.076(5) Uani 1 1 d G . . 
H15A H 0.0586 0.6197 0.4067 0.091 Uiso 1 1 calc R . . 
C16 C -0.0839(10) 0.7051(8) 0.2878(8) 0.058(4) Uani 1 1 d G . . 
H16A H -0.0672 0.6308 0.2741 0.070 Uiso 1 1 calc R . . 
C21 C -0.6438(7) 1.0191(9) 0.2218(7) 0.040(3) Uani 1 1 d G . . 
C22 C -0.7013(9) 0.9460(7) 0.2948(7) 0.057(4) Uani 1 1 d GD . . 
C23 C -0.8084(9) 1.0107(10) 0.3291(6) 0.063(5) Uani 1 1 d G . . 
H23A H -0.8469 0.9618 0.3779 0.075 Uiso 1 1 calc R . . 
C24 C -0.8580(7) 1.1485(11) 0.2905(8) 0.056(4) Uani 1 1 d G . . 
C25 C -0.8005(8) 1.2216(7) 0.2175(8) 0.056(4) Uani 1 1 d G . . 
H25A H -0.8336 1.3138 0.1917 0.067 Uiso 1 1 calc R . . 
C26 C -0.6934(8) 1.1569(8) 0.1832(6) 0.046(3) Uani 1 1 d G . . 
H26A H -0.6549 1.2058 0.1344 0.055 Uiso 1 1 calc R . . 
C27 C -0.5272(13) 0.9531(14) 0.1846(10) 0.040(3) Uani 1 1 d . . . 
C28 C -0.9787(17) 1.212(2) 0.3299(15) 0.092(6) Uani 1 1 d . . . 
H28A H -1.0043 1.3068 0.2983 0.138 Uiso 1 1 calc R . . 
H28B H -0.9607 1.1812 0.4023 0.138 Uiso 1 1 calc R . . 
H28C H -1.0467 1.1877 0.3137 0.138 Uiso 1 1 calc R . . 
C31 C -0.3389(9) 0.4412(8) 0.2181(7) 0.045(4) Uani 1 1 d G . . 
C32 C -0.3064(9) 0.3833(9) 0.3234(7) 0.047(4) Uani 1 1 d GD . . 
C33 C -0.3385(10) 0.2755(9) 0.3822(6) 0.066(5) Uani 1 1 d G . . 
H33A H -0.3167 0.2367 0.4526 0.079 Uiso 1 1 calc R . . 
C34 C -0.4031(10) 0.2255(8) 0.3357(9) 0.073(6) Uani 1 1 d G . . 
C35 C -0.4355(10) 0.2833(10) 0.2304(9) 0.066(5) Uani 1 1 d G . . 
H35A H -0.4788 0.2499 0.1993 0.080 Uiso 1 1 calc R . . 
C36 C -0.4035(9) 0.3912(10) 0.1716(7) 0.103(8) Uani 1 1 d G . . 
H36A H -0.4252 0.4299 0.1012 0.123 Uiso 1 1 calc R . . 
C37 C -0.3105(15) 0.5597(14) 0.1529(14) 0.057(4) Uani 1 1 d . . . 
C38 C -0.435(2) 0.107(2) 0.4040(18) 0.121(9) Uani 1 1 d . . . 
H38A H -0.4052 0.0825 0.4738 0.181 Uiso 1 1 calc R . . 
H38B H -0.3935 0.0333 0.3866 0.181 Uiso 1 1 calc R . . 
H38C H -0.5261 0.1296 0.3946 0.181 Uiso 1 1 calc R . . 
N11 N -0.1029(7) 0.7771(8) 0.0316(6) 0.044(3) Uani 1 1 d G . . 
C41 C -0.0275(9) 0.6445(7) 0.0581(6) 0.056(4) Uani 1 1 d G . . 
H41A H -0.0476 0.5780 0.1082 0.067 Uiso 1 1 calc R . . 
C42 C 0.0779(8) 0.6114(7) 0.0095(8) 0.057(4) Uani 1 1 d G . . 
H42A H 0.1284 0.5227 0.0272 0.068 Uiso 1 1 calc R . . 
C43 C 0.1080(8) 0.7108(10) -0.0654(7) 0.064(5) Uani 1 1 d G . . 
H43A H 0.1785 0.6886 -0.0979 0.077 Uiso 1 1 calc R . . 
C44 C 0.0325(9) 0.8433(9) -0.0919(6) 0.055(4) Uani 1 1 d G . . 
H44A H 0.0526 0.9099 -0.1421 0.066 Uiso 1 1 calc R . . 
C45 C -0.0729(8) 0.8765(6) -0.0434(6) 0.045(4) Uani 1 1 d G . . 
C46 C -0.1529(12) 1.0121(13) -0.0623(9) 0.036(3) Uani 1 1 d . . . 
C47 C -0.1284(14) 1.1207(15) -0.1308(11) 0.050(4) Uani 1 1 d . . . 
H47A H -0.0592 1.1072 -0.1663 0.060 Uiso 1 1 calc R . . 
C48 C -0.2044(17) 1.2457(17) -0.1462(11) 0.062(5) Uani 1 1 d . . . 
H48A H -0.1872 1.3180 -0.1912 0.074 Uiso 1 1 calc R . . 
C49 C -0.3043(16) 1.2639(16) -0.0960(11) 0.058(4) Uani 1 1 d . . . 
H49A H -0.3581 1.3491 -0.1061 0.070 Uiso 1 1 calc R . . 
N12 N -0.2517(10) 1.0312(11) -0.0116(8) 0.039(3) Uani 1 1 d . . . 
N61 N -0.3075(13) 1.6061(13) -0.4390(12) 0.065(4) Uani 1 1 d . . . 
O61 O -0.2006(17) 1.5418(14) -0.2885(13) 0.116(6) Uani 1 1 d . . . 
C62 C -0.3609(17) 1.511(2) -0.4151(17) 0.102(7) Uani 1 1 d . . . 
H62A H -0.3332 1.4507 -0.3446 0.153 Uiso 1 1 calc R . . 
H62B H -0.3339 1.4626 -0.4566 0.153 Uiso 1 1 calc R . . 
H62C H -0.4527 1.5527 -0.4273 0.153 Uiso 1 1 calc R . . 
C61 C -0.232(3) 1.617(2) -0.380(2) 0.104(7) Uani 1 1 d . . . 
H61A H -0.2003 1.6850 -0.4063 0.125 Uiso 1 1 calc R . . 
C63 C -0.343(2) 1.700(2) -0.5440(16) 0.109(8) Uani 1 1 d . . . 
H63A H -0.3031 1.7633 -0.5565 0.164 Uiso 1 1 calc R . . 
H63B H -0.4348 1.7450 -0.5587 0.164 Uiso 1 1 calc R . . 
H63C H -0.3159 1.6536 -0.5869 0.164 Uiso 1 1 calc R . . 
C50 C -0.3270(14) 1.1554(13) -0.0291(12) 0.055(4) Uani 1 1 d . . . 
H50A H -0.3974 1.1689 0.0051 0.066 Uiso 1 1 calc R . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Bi1 C11 2.250(7) . ? 
Bi1 O32 2.388(8) . ? 
Bi1 O21 2.464(9) . ? 
Bi1 N11 2.490(6) . ? 
Bi1 N12 2.534(10) . ?
Bi1 O22 2.594(9) . ? 
O21 C27 1.272(15) . ? 
O22 C27 1.281(16) . ? 
O23 C22 1.368(12) . ? 
O32 C37 1.292(16) . ? 
O31 C37 1.220(19) . ? 
O33 C32 1.307(15) . ? 
C11 C12 1.3900 . ? 
C11 C16 1.3900 . ? 
C12 C13 1.3900 . ? 
C13 C14 1.3900 . ? 
C14 C15 1.3900 . ? 
C15 C16 1.3900 . ? 
C21 C22 1.3900 . ? 
C21 C26 1.3900 . ? 
C21 C27 1.493(14) . ? 
C22 C23 1.3900 . ? 
C23 C24 1.3900 . ? 
C24 C25 1.3900 . ? 
C24 C28 1.532(17) . ? 
C25 C26 1.3900 . ? 
C31 C32 1.3900 . ? 
C31 C36 1.3900 . ? 
C31 C37 1.487(16) . ? 
C32 C33 1.3900 . ? 
C33 C34 1.3900 . ? 
C34 C35 1.3900 . ? 
C34 C38 1.522(18) . ? 
C35 C36 1.3900 . ? 
N11 C41 1.3900 . ? 
N11 C45 1.3900 . ? 
C41 C42 1.3900 . ? 
C42 C43 1.3900 . ? 
C43 C44 1.3900 . ? 
C44 C45 1.3900 . ? 
C45 C46 1.453(14) . ? 
C46 N12 1.330(15) . ? 
C46 C47 1.392(18) . ? 
C47 C48 1.35(2) . ? 
C48 C49 1.33(2) . ? 
C49 C50 1.37(2) . ? 
N12 C50 1.336(16) . ? 
N61 C61 1.28(2) . ? 
N61 C62 1.38(2) . ? 
N61 C63 1.44(2) . ? 
O61 C61 1.23(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 
C11 Bi1 O32 84.1(3) . . ? 
C11 Bi1 O21 86.8(3) . . ? 
O32 Bi1 O21 129.3(3) . . ? 
C11 Bi1 N11 83.9(3) . . ? 
O32 Bi1 N11 86.3(3) . . ? 
O21 Bi1 N11 141.9(3) . . ? 
C11 Bi1 N12 86.2(3) . . ? 
O32 Bi1 N12 150.5(3) . . ? 
O21 Bi1 N12 77.7(3) . . ? 
N11 Bi1 N12 64.9(3) . . ? 
C11 Bi1 O22 86.2(3) . . ? 
O32 Bi1 O22 77.5(3) . . ? 
O21 Bi1 O22 52.1(3) . . ? 
N11 Bi1 O22 161.8(3) . . ? 
N12 Bi1 O22 129.6(3) . . ? 
C27 O21 Bi1 96.3(8) . . ? 
C27 O22 Bi1 90.0(8) . . ? 
C37 O32 Bi1 107.9(9) . . ? 
C12 C11 C16 120.0 . . ? 
C12 C11 Bi1 119.4(5) . . ? 
C16 C11 Bi1 120.6(5) . . ? 
C13 C12 C11 120.0 . . ? 
C12 C13 C14 120.0 . . ? 
C15 C14 C13 120.0 . . ? 
C14 C15 C16 120.0 . . ? 
C15 C16 C11 120.0 . . ? 
C22 C21 C26 120.0 . . ? 
C22 C21 C27 121.5(8) . . ? 
C26 C21 C27 118.5(8) . . ? 
O23 C22 C23 117.5(8) . . ? 
O23 C22 C21 122.4(8) . . ? 
C23 C22 C21 120.0 . . ? 
C22 C23 C24 120.0 . . ? 
C25 C24 C23 120.0 . . ? 
C25 C24 C28 123.3(10) . . ? 
C23 C24 C28 116.6(10) . . ? 
C26 C25 C24 120.0 . . ? 
C25 C26 C21 120.0 . . ? 
O21 C27 O22 121.4(12) . . ? 
O21 C27 C21 120.1(11) . . ? 
O22 C27 C21 118.5(11) . . ? 
C32 C31 C36 120.0 . . ? 
C32 C31 C37 121.6(9) . . ? 
C36 C31 C37 118.3(9) . . ? 
O33 C32 C31 123.6(9) . . ? 
O33 C32 C33 116.4(9) . . ? 
C31 C32 C33 120.0 . . ? 
C34 C33 C32 120.0 . . ? 
C33 C34 C35 120.0 . . ? 
C33 C34 C38 117.6(12) . . ? 
C35 C34 C38 122.4(12) . . ? 
C36 C35 C34 120.0 . . ? 
C35 C36 C31 120.0 . . ? 
O31 C37 O32 122.6(14) . . ? 
O31 C37 C31 120.8(13) . . ? 
O32 C37 C31 116.5(14) . . ? 
C41 N11 C45 120.0 . . ? 
C41 N11 Bi1 119.7(4) . . ? 
C45 N11 Bi1 119.7(4) . . ? 
N11 C41 C42 120.0 . . ? 
C41 C42 C43 120.0 . . ? 
C44 C43 C42 120.0 . . ? 
C43 C44 C45 120.0 . . ? 
C44 C45 N11 120.0 . . ? 
C44 C45 C46 123.7(7) . . ? 
N11 C45 C46 116.2(7) . . ? 
N12 C46 C47 119.8(12) . . ? 
N12 C46 C45 118.1(11) . . ? 
C47 C46 C45 122.1(11) . . ? 
C48 C47 C46 120.5(13) . . ? 
C49 C48 C47 119.2(15) . . ? 
C48 C49 C50 119.3(16) . . ? 
C46 N12 C50 118.7(12) . . ? 
C46 N12 Bi1 119.7(9) . . ? 
C50 N12 Bi1 121.2(9) . . ? 
C61 N61 C62 127.5(18) . . ? 
C61 N61 C63 119.5(17) . . ? 
C62 N61 C63 113.0(17) . . ? 
O61 C61 N61 122.3(19) . . ? 
N12 C50 C49 122.4(14) . . ? 
 
_diffrn_measured_fraction_theta_max    0.832 
_diffrn_reflns_theta_full              28.37 
_diffrn_measured_fraction_theta_full   0.832 
_refine_diff_density_max    1.632 
_refine_diff_density_min   -1.972 
_refine_diff_density_rms    0.182 
