data_rbchan
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C24 H18 O4'
_chemical_formula_weight          370.38
 
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'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P21/c
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    4.967(5)
_cell_length_b                    27.181(14)
_cell_length_c                    7.764(7)
_cell_angle_alpha                 90.00
_cell_angle_beta                  117.55(6)
_cell_angle_gamma                 90.00
_cell_volume                      929.3(13)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           .31
_exptl_crystal_size_mid           .30
_exptl_crystal_size_min           .29
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.324
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              388
_exptl_absorpt_coefficient_mu     0.090
_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       293(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             3448
_diffrn_reflns_av_R_equivalents   0.1018
_diffrn_reflns_av_sigmaI/netI     0.2291
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -34
_diffrn_reflns_limit_k_max        25
_diffrn_reflns_limit_l_min        -8
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          4.69
_diffrn_reflns_theta_max          29.49
_reflns_number_total              2580
_reflns_number_gt                 1750
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0000P)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          1750
_refine_ls_number_parameters      127
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.2075
_refine_ls_R_factor_gt            0.0532
_refine_ls_wR_factor_ref          0.0967
_refine_ls_wR_factor_gt           0.0538
_refine_ls_goodness_of_fit_ref    0.735
_refine_ls_restrained_S_all       0.735
_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
O1 O 0.3719(5) 0.07980(8) 0.4747(3) 0.0732(7) Uani 1 1 d . . .
O2 O -0.0579(4) 0.14077(8) 0.3457(3) 0.0801(8) Uani 1 1 d . . .
H1 H 0.0563 0.1198 0.3398 0.120 Uiso 1 1 d R . .
C2 C 1.4095(6) 0.04130(11) 1.0653(4) 0.0475(8) Uani 1 1 d . . .
H4 H 1.3500 0.0688 1.1106 0.057 Uiso 1 1 calc R . .
C4 C 1.2162(6) 0.02202(10) 0.8831(4) 0.0396(7) Uani 1 1 d . . .
C5 C 0.4505(6) 0.16323(12) 0.8607(4) 0.0528(8) Uani 1 1 d . . .
H5 H 0.6323 0.1521 0.9616 0.063 Uiso 1 1 calc R . .
C6 C -0.0867(7) 0.19740(12) 0.5659(5) 0.0624(9) Uani 1 1 d . . .
H6 H -0.2682 0.2092 0.4671 0.075 Uiso 1 1 calc R . .
C7 C 0.9168(5) 0.04365(11) 0.7539(4) 0.0468(8) Uani 1 1 d . . .
H7 H 0.8019 0.0271 0.6377 0.056 Uiso 1 1 calc R . .
C9 C 0.0642(6) 0.15946(11) 0.5286(4) 0.0490(8) Uani 1 1 d . . .
C12 C 0.3426(6) 0.14169(10) 0.6789(4) 0.0421(7) Uani 1 1 d . . .
C14 C 1.3096(6) -0.01985(12) 0.8202(4) 0.0484(8) Uani 1 1 d . . .
H10 H 1.1816 -0.0335 0.6999 0.058 Uiso 1 1 calc R . .
C21 C 0.7940(5) 0.08335(11) 0.7834(4) 0.0441(7) Uani 1 1 d . . .
H15 H 0.8969 0.1007 0.8989 0.053 Uiso 1 1 calc R . .
C23 C 0.0292(7) 0.21753(13) 0.7467(5) 0.0731(10) Uani 1 1 d . . .
H17 H -0.0734 0.2432 0.7699 0.088 Uiso 1 1 calc R . .
C26 C 0.4944(6) 0.10077(10) 0.6356(4) 0.0452(7) Uani 1 1 d . . .
C34 C 0.2962(7) 0.20038(13) 0.8955(5) 0.0710(10) Uani 1 1 d . . .
H23 H 0.3713 0.2140 1.0191 0.085 Uiso 1 1 calc R . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
O1 0.0662(14) 0.0821(19) 0.0523(14) -0.0155(14) 0.0114(11) 0.0163(13)
O2 0.0705(14) 0.097(2) 0.0486(14) 0.0014(14) 0.0065(11) 0.0268(13)
C2 0.0496(17) 0.0452(19) 0.0489(19) -0.0051(15) 0.0238(15) 0.0003(14)
C4 0.0420(15) 0.0371(17) 0.0376(17) -0.0018(14) 0.0167(13) -0.0058(13)
C5 0.0384(16) 0.057(2) 0.057(2) -0.0058(18) 0.0166(15) -0.0024(15)
C6 0.059(2) 0.054(2) 0.069(2) 0.0228(19) 0.0248(18) 0.0173(17)
C7 0.0405(16) 0.051(2) 0.0448(18) 0.0006(15) 0.0163(14) 0.0005(14)
C9 0.0512(18) 0.0439(19) 0.0428(18) 0.0076(15) 0.0139(14) 0.0015(15)
C12 0.0399(15) 0.0408(18) 0.0421(18) 0.0063(14) 0.0161(14) -0.0056(13)
C14 0.0500(17) 0.0468(19) 0.0382(18) -0.0056(15) 0.0119(14) -0.0025(14)
C21 0.0365(15) 0.0482(19) 0.0386(17) 0.0003(15) 0.0096(13) -0.0055(14)
C23 0.066(2) 0.067(3) 0.085(3) -0.002(2) 0.034(2) 0.0113(18)
C26 0.0501(18) 0.0422(19) 0.0414(18) -0.0018(15) 0.0195(15) -0.0089(14)
C34 0.071(2) 0.068(3) 0.072(2) -0.028(2) 0.032(2) -0.0086(19)
 
_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
O1 C26 1.246(3) . ?
O2 C9 1.359(3) . ?
O2 H1 0.8201 . ?
C2 C14 1.389(4) 3_857 ?
C2 C4 1.393(4) . ?
C2 H4 0.9300 . ?
C4 C14 1.400(4) . ?
C4 C7 1.478(4) . ?
C5 C34 1.368(4) . ?
C5 C12 1.387(4) . ?
C5 H5 0.9300 . ?
C6 C23 1.361(4) . ?
C6 C9 1.382(4) . ?
C6 H6 0.9300 . ?
C7 C21 1.311(3) . ?
C7 H7 0.9300 . ?
C9 C12 1.419(4) . ?
C12 C26 1.467(4) . ?
C14 C2 1.389(4) 3_857 ?
C14 H10 0.9300 . ?
C21 C26 1.475(4) . ?
C21 H15 0.9300 . ?
C23 C34 1.376(4) . ?
C23 H17 0.9300 . ?
C34 H23 0.9300 . ?
 
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
C9 O2 H1 109.4 . . ?
C14 C2 C4 120.6(3) 3_857 . ?
C14 C2 H4 119.7 3_857 . ?
C4 C2 H4 119.7 . . ?
C2 C4 C14 118.4(3) . . ?
C2 C4 C7 123.0(3) . . ?
C14 C4 C7 118.6(3) . . ?
C34 C5 C12 121.6(3) . . ?
C34 C5 H5 119.2 . . ?
C12 C5 H5 119.2 . . ?
C23 C6 C9 120.3(3) . . ?
C23 C6 H6 119.9 . . ?
C9 C6 H6 119.9 . . ?
C21 C7 C4 127.8(3) . . ?
C21 C7 H7 116.1 . . ?
C4 C7 H7 116.1 . . ?
O2 C9 C6 118.3(3) . . ?
O2 C9 C12 121.8(3) . . ?
C6 C9 C12 119.9(3) . . ?
C5 C12 C9 117.7(3) . . ?
C5 C12 C26 123.8(3) . . ?
C9 C12 C26 118.6(3) . . ?
C2 C14 C4 121.0(3) 3_857 . ?
C2 C14 H10 119.5 3_857 . ?
C4 C14 H10 119.5 . . ?
C7 C21 C26 120.8(3) . . ?
C7 C21 H15 119.6 . . ?
C26 C21 H15 119.6 . . ?
C6 C23 C34 120.9(3) . . ?
C6 C23 H17 119.6 . . ?
C34 C23 H17 119.6 . . ?
O1 C26 C12 120.8(3) . . ?
O1 C26 C21 118.8(3) . . ?
C12 C26 C21 120.4(3) . . ?
C5 C34 C23 119.6(3) . . ?
C5 C34 H23 120.2 . . ?
C23 C34 H23 120.2 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C14 C2 C4 C14 1.1(5) 3_857 . . . ?
C14 C2 C4 C7 -179.1(2) 3_857 . . . ?
C2 C4 C7 C21 2.6(5) . . . . ?
C14 C4 C7 C21 -177.6(3) . . . . ?
C23 C6 C9 O2 -179.3(3) . . . . ?
C23 C6 C9 C12 -0.6(4) . . . . ?
C34 C5 C12 C9 -0.1(4) . . . . ?
C34 C5 C12 C26 -178.0(3) . . . . ?
O2 C9 C12 C5 179.6(3) . . . . ?
C6 C9 C12 C5 0.9(4) . . . . ?
O2 C9 C12 C26 -2.4(4) . . . . ?
C6 C9 C12 C26 178.9(3) . . . . ?
C2 C4 C14 C2 -1.1(5) . . . 3_857 ?
C7 C4 C14 C2 179.1(2) . . . 3_857 ?
C4 C7 C21 C26 178.2(3) . . . . ?
C9 C6 C23 C34 -0.5(5) . . . . ?
C5 C12 C26 O1 173.0(3) . . . . ?
C9 C12 C26 O1 -4.9(4) . . . . ?
C5 C12 C26 C21 -6.2(4) . . . . ?
C9 C12 C26 C21 175.9(3) . . . . ?
C7 C21 C26 O1 -6.5(4) . . . . ?
C7 C21 C26 C12 172.7(2) . . . . ?
C12 C5 C34 C23 -0.9(5) . . . . ?
C6 C23 C34 C5 1.2(5) . . . . ?
 
_diffrn_measured_fraction_theta_max    0.980
_diffrn_reflns_theta_full              29.49
_diffrn_measured_fraction_theta_full   0.980
_refine_diff_density_max    0.091
_refine_diff_density_min   -0.094
_refine_diff_density_rms    0.024
