 
data_1corr 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C31 H27 Bi N2 O7' 
_chemical_formula_weight          748.53 
 
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            '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                    15.979(3) 
_cell_length_b                    15.472(3) 
_cell_length_c                    12.295(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  108.13(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      2888.9(10) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     5485 
_cell_measurement_theta_min       4.523 
_cell_measurement_theta_max       4.523 
 
_exptl_crystal_description        bloc 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.21 
_exptl_crystal_size_mid           0.14 
_exptl_crystal_size_min           0.09 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.721 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1464 
_exptl_absorpt_coefficient_mu     6.153 
_exptl_absorpt_correction_type    'multi-scan'  
_exptl_absorpt_correction_T_min   0.359 
_exptl_absorpt_correction_T_max   0.575  
_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             34904 
_diffrn_reflns_av_R_equivalents   0.0509 
_diffrn_reflns_av_sigmaI/netI     0.0457 
_diffrn_reflns_limit_h_min        -21 
_diffrn_reflns_limit_h_max        20 
_diffrn_reflns_limit_k_min        -20 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          1.88 
_diffrn_reflns_theta_max          28.30 
_reflns_number_total              7012 
_reflns_number_gt                 3805 
_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)+(0.0382P)²+4.6912P] 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          7012 
_refine_ls_number_parameters      373 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0908 
_refine_ls_R_factor_gt            0.0334 
_refine_ls_wR_factor_ref          0.0996 
_refine_ls_wR_factor_gt           0.0722 
_refine_ls_goodness_of_fit_ref    1.034 
_refine_ls_restrained_S_all       1.034 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Bi1 Bi 0.418877(14) 0.502768(15) 0.331536(15) 0.04346(8) Uani 1 1 d . . . 
N11 N 0.5028(3) 0.5959(3) 0.2322(4) 0.0481(12) Uani 1 1 d . . . 
N12 N 0.3640(3) 0.4934(3) 0.1139(4) 0.0474(12) Uani 1 1 d . . . 
O11 O 0.2944(3) 0.3897(3) 0.3060(4) 0.0640(12) Uani 1 1 d . . . 
O12 O 0.3290(3) 0.4735(3) 0.4571(4) 0.0579(12) Uani 1 1 d D . . 
O13 O 0.2425(4) 0.4664(4) 0.6009(4) 0.0797(16) Uani 1 1 d D . . 
H13B H 0.284(2) 0.476(5) 0.576(3) 0.096 Uiso 1 1 d D . . 
O21 O 0.4451(3) 0.6296(4) 0.6371(4) 0.0740(14) Uani 1 1 d . . . 
O22 O 0.4750(3) 0.5943(3) 0.4799(3) 0.0497(11) Uani 1 1 d . . . 
O23 O 0.3283(3) 0.6058(3) 0.2788(3) 0.0548(11) Uani 1 1 d . . . 
C11 C 0.2227(4) 0.3652(4) 0.4463(5) 0.0513(15) Uani 1 1 d . . . 
C12 C 0.2050(5) 0.3946(5) 0.5432(5) 0.0590(18) Uani 1 1 d . . . 
C13 C 0.1438(5) 0.3507(5) 0.5829(6) 0.071(2) Uani 1 1 d . . . 
H13A H 0.1328 0.3707 0.6484 0.085 Uiso 1 1 calc R . . 
C14 C 0.0998(5) 0.2796(6) 0.5286(8) 0.079(2) Uani 1 1 d . . . 
C15 C 0.1188(6) 0.2507(5) 0.4322(8) 0.087(3) Uani 1 1 d . . . 
H15A H 0.0902 0.2020 0.3941 0.105 Uiso 1 1 calc R . . 
C16 C 0.1789(5) 0.2925(5) 0.3916(7) 0.070(2) Uani 1 1 d . . . 
H16A H 0.1903 0.2716 0.3267 0.085 Uiso 1 1 calc R . . 
C17 C 0.2848(4) 0.4109(4) 0.3988(5) 0.0495(15) Uani 1 1 d . . . 
C18 C 0.0309(6) 0.2343(7) 0.5697(10) 0.124(4) Uani 1 1 d . . . 
H18A H 0.0269 0.2622 0.6376 0.186 Uiso 1 1 calc R . . 
H18B H 0.0473 0.1749 0.5863 0.186 Uiso 1 1 calc R . . 
H18C H -0.0252 0.2372 0.5111 0.186 Uiso 1 1 calc R . . 
C21 C 0.3442(4) 0.6765(4) 0.4635(5) 0.0453(14) Uani 1 1 d . . . 
C22 C 0.3044(4) 0.6651(4) 0.3429(5) 0.0478(15) Uani 1 1 d . . . 
C23 C 0.2344(4) 0.7198(4) 0.2866(5) 0.0552(16) Uani 1 1 d . . . 
H23A H 0.2095 0.7142 0.2077 0.066 Uiso 1 1 calc R . . 
C24 C 0.2004(4) 0.7816(4) 0.3425(6) 0.0576(17) Uani 1 1 d . . . 
C25 C 0.2375(5) 0.7892(4) 0.4609(6) 0.0617(18) Uani 1 1 d . . . 
H25A H 0.2151 0.8293 0.5009 0.074 Uiso 1 1 calc R . . 
C26 C 0.3074(5) 0.7373(4) 0.5186(5) 0.0549(16) Uani 1 1 d . . . 
H26A H 0.3308 0.7432 0.5976 0.066 Uiso 1 1 calc R . . 
C27 C 0.4239(4) 0.6302(4) 0.5318(5) 0.0493(15) Uani 1 1 d . . . 
C28 C 0.1269(5) 0.8394(5) 0.2758(6) 0.073(2) Uani 1 1 d . . . 
H28A H 0.1117 0.8786 0.3271 0.110 Uiso 1 1 calc R . . 
H28B H 0.0765 0.8050 0.2369 0.110 Uiso 1 1 calc R . . 
H28C H 0.1456 0.8717 0.2208 0.110 Uiso 1 1 calc R . . 
C31 C 0.5693(4) 0.6456(4) 0.2893(6) 0.0606(18) Uani 1 1 d . . . 
H31A H 0.5891 0.6423 0.3687 0.073 Uiso 1 1 calc R . . 
C32 C 0.6108(5) 0.7027(5) 0.2349(8) 0.075(2) Uani 1 1 d . . . 
H32A H 0.6569 0.7374 0.2773 0.090 Uiso 1 1 calc R . . 
C33 C 0.5827(5) 0.7066(5) 0.1192(8) 0.075(2) Uani 1 1 d . . . 
H33A H 0.6094 0.7447 0.0817 0.090 Uiso 1 1 calc R . . 
C34 C 0.5143(5) 0.6541(4) 0.0561(7) 0.0596(18) Uani 1 1 d . . . 
C35 C 0.4748(4) 0.5989(4) 0.1160(5) 0.0480(15) Uani 1 1 d . . . 
C36 C 0.4021(4) 0.5448(4) 0.0540(5) 0.0460(15) Uani 1 1 d . . . 
C37 C 0.3721(5) 0.5485(5) -0.0658(5) 0.0582(18) Uani 1 1 d . . . 
C38 C 0.3004(5) 0.4955(5) -0.1217(5) 0.069(2) Uani 1 1 d . . . 
H38A H 0.2797 0.4945 -0.2013 0.082 Uiso 1 1 calc R . . 
C39 C 0.2614(5) 0.4462(5) -0.0616(6) 0.074(2) Uani 1 1 d . . . 
H39A H 0.2123 0.4129 -0.0984 0.089 Uiso 1 1 calc R . . 
C40 C 0.2963(5) 0.4463(5) 0.0570(5) 0.0627(19) Uani 1 1 d . . . 
H40A H 0.2701 0.4110 0.0983 0.075 Uiso 1 1 calc R . . 
C41 C 0.4803(6) 0.6544(5) -0.0680(7) 0.074(2) Uani 1 1 d . . . 
H41A H 0.5065 0.6903 -0.1087 0.089 Uiso 1 1 calc R . . 
C42 C 0.4137(6) 0.6053(5) -0.1249(6) 0.072(2) Uani 1 1 d . . . 
H42A H 0.3935 0.6076 -0.2044 0.086 Uiso 1 1 calc R . . 
O51 O 0.0359(7) 0.0634(7) 0.3195(12) 0.239(6) Uani 1 1 d . . . 
C53 C -0.1013(11) 0.0172(9) 0.3303(15) 0.196(9) Uani 1 1 d . . . 
H53A H -0.0719 0.0157 0.4113 0.294 Uiso 1 1 calc R . . 
H53B H -0.1245 -0.0391 0.3047 0.294 Uiso 1 1 calc R . . 
H53C H -0.1485 0.0583 0.3139 0.294 Uiso 1 1 calc R . . 
C51 C -0.0375(11) 0.0429(9) 0.270(2) 0.178(8) Uani 1 1 d . . . 
C52 C -0.0733(12) 0.0452(12) 0.1480(18) 0.237(10) Uani 1 1 d . . . 
H52A H -0.0282 0.0618 0.1157 0.355 Uiso 1 1 calc R . . 
H52B H -0.1206 0.0863 0.1262 0.355 Uiso 1 1 calc R . . 
H52C H -0.0952 -0.0111 0.1202 0.355 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 O23 2.115(4) . ? 
Bi1 O22 2.263(4) . ? 
Bi1 O12 2.455(4) . ? 
Bi1 N11 2.527(5) . ? 
Bi1 N12 2.548(4) . ? 
Bi1 O11 2.594(5) . ? 
N11 C31 1.322(8) . ? 
N11 C35 1.359(7) . ? 
N12 C40 1.313(8) . ? 
N12 C36 1.350(8) . ? 
O11 C17 1.241(7) . ? 
O12 C17 1.279(7) . ? 
O13 C12 1.353(8) . ? 
O21 C27 1.232(6) . ? 
O22 C27 1.307(7) . ? 
O23 C22 1.340(7) . ? 
C11 C12 1.384(8) . ? 
C11 C16 1.384(9) . ? 
C11 C17 1.480(8) . ? 
C12 C13 1.397(9) . ? 
C13 C14 1.363(10) . ? 
C14 C15 1.386(11) . ? 
C14 C18 1.519(10) . ? 
C15 C16 1.374(10) . ? 
C21 C26 1.394(8) . ? 
C21 C22 1.431(8) . ? 
C21 C27 1.475(8) . ? 
C22 C23 1.402(9) . ? 
C23 C24 1.384(9) . ? 
C24 C25 1.395(9) . ? 
C24 C28 1.500(9) . ? 
C25 C26 1.378(9) . ? 
C31 C32 1.394(9) . ? 
C32 C33 1.353(11) . ? 
C33 C34 1.388(10) . ? 
C34 C35 1.400(8) . ? 
C34 C41 1.452(10) . ? 
C35 C36 1.442(9) . ? 
C36 C37 1.400(8) . ? 
C37 C38 1.403(10) . ? 
C37 C42 1.429(10) . ? 
C38 C39 1.343(10) . ? 
C39 C40 1.389(9) . ? 
C41 C42 1.317(11) . ? 
O51 C51 1.184(14) . ? 
C53 C51 1.49(2) . ? 
C51 C52 1.43(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 
O23 Bi1 O22 80.66(16) . . ? 
O23 Bi1 O12 81.55(16) . . ? 
O22 Bi1 O12 76.77(14) . . ? 
O23 Bi1 N11 80.66(17) . . ? 
O22 Bi1 N11 84.01(15) . . ? 
O12 Bi1 N11 155.64(15) . . ? 
O23 Bi1 N12 75.03(15) . . ? 
O22 Bi1 N12 143.40(15) . . ? 
O12 Bi1 N12 124.93(16) . . ? 
N11 Bi1 N12 65.52(16) . . ? 
O23 Bi1 O11 92.57(17) . . ? 
O22 Bi1 O11 128.06(14) . . ? 
O12 Bi1 O11 51.34(14) . . ? 
N11 Bi1 O11 145.95(15) . . ? 
N12 Bi1 O11 80.47(15) . . ? 
C31 N11 C35 119.0(6) . . ? 
C31 N11 Bi1 122.3(4) . . ? 
C35 N11 Bi1 118.5(4) . . ? 
C40 N12 C36 118.2(5) . . ? 
C40 N12 Bi1 123.3(4) . . ? 
C36 N12 Bi1 118.3(4) . . ? 
C17 O11 Bi1 91.1(4) . . ? 
C17 O12 Bi1 96.7(4) . . ? 
C27 O22 Bi1 120.6(4) . . ? 
C22 O23 Bi1 129.0(4) . . ? 
C12 C11 C16 118.6(6) . . ? 
C12 C11 C17 121.6(6) . . ? 
C16 C11 C17 119.8(6) . . ? 
O13 C12 C11 123.0(6) . . ? 
O13 C12 C13 117.4(6) . . ? 
C11 C12 C13 119.5(7) . . ? 
C14 C13 C12 122.2(7) . . ? 
C13 C14 C15 117.5(7) . . ? 
C13 C14 C18 121.8(9) . . ? 
C15 C14 C18 120.7(9) . . ? 
C16 C15 C14 121.5(8) . . ? 
C15 C16 C11 120.7(7) . . ? 
O11 C17 O12 120.7(6) . . ? 
O11 C17 C11 121.8(6) . . ? 
O12 C17 C11 117.5(5) . . ? 
C26 C21 C22 117.9(6) . . ? 
C26 C21 C27 118.1(5) . . ? 
C22 C21 C27 123.9(5) . . ? 
O23 C22 C23 116.9(5) . . ? 
O23 C22 C21 125.3(6) . . ? 
C23 C22 C21 117.8(6) . . ? 
C24 C23 C22 123.3(6) . . ? 
C23 C24 C25 118.1(6) . . ? 
C23 C24 C28 120.1(6) . . ? 
C25 C24 C28 121.8(6) . . ? 
C26 C25 C24 120.1(6) . . ? 
C25 C26 C21 122.7(6) . . ? 
O21 C27 O22 120.0(6) . . ? 
O21 C27 C21 120.6(6) . . ? 
O22 C27 C21 119.2(5) . . ? 
N11 C31 C32 122.5(7) . . ? 
C33 C32 C31 118.7(8) . . ? 
C32 C33 C34 120.5(7) . . ? 
C33 C34 C35 117.9(7) . . ? 
C33 C34 C41 123.9(7) . . ? 
C35 C34 C41 118.1(7) . . ? 
N11 C35 C34 121.2(7) . . ? 
N11 C35 C36 118.9(5) . . ? 
C34 C35 C36 119.8(6) . . ? 
N12 C36 C37 122.2(6) . . ? 
N12 C36 C35 118.6(5) . . ? 
C37 C36 C35 119.2(6) . . ? 
C36 C37 C38 116.9(6) . . ? 
C36 C37 C42 119.9(7) . . ? 
C38 C37 C42 123.2(7) . . ? 
C39 C38 C37 120.7(6) . . ? 
C38 C39 C40 118.3(8) . . ? 
N12 C40 C39 123.7(7) . . ? 
C42 C41 C34 122.2(7) . . ? 
C41 C42 C37 120.8(7) . . ? 
O51 C51 C52 123(2) . . ? 
O51 C51 C53 123(2) . . ? 
C52 C51 C53 114.6(14) . . ? 
 
_diffrn_measured_fraction_theta_max    0.974 
_diffrn_reflns_theta_full              28.30 
_diffrn_measured_fraction_theta_full   0.974 
_refine_diff_density_max    1.234 
_refine_diff_density_min   -0.703 
_refine_diff_density_rms    0.110 
