 
data_peng 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C18 H15 Br O2' 
_chemical_formula_weight          343.21 
 
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' 
 'Br'  'Br'  -0.2901   2.4595 
 '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                    9.2983(19) 
_cell_length_b                    9.5365(19) 
_cell_length_c                    10.425(2) 
_cell_angle_alpha                 107.87(3) 
_cell_angle_beta                  104.21(3) 
_cell_angle_gamma                 109.44(3) 
_cell_volume                      764.9(3) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     3834
_cell_measurement_theta_min       6.81
_cell_measurement_theta_max       55.07
 
_exptl_crystal_description        block
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.1
_exptl_crystal_size_min           0.1
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.490 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              348 
_exptl_absorpt_coefficient_mu     2.688 
_exptl_absorpt_correction_type    ? 
_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   Rigaku
_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             7123 
_diffrn_reflns_av_R_equivalents   0.0347 
_diffrn_reflns_av_sigmaI/netI     0.0491 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          3.41 
_diffrn_reflns_theta_max          27.47 
_reflns_number_total              3437 
_reflns_number_gt                 2204 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_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)+(0.1167P)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      SHELXL 
_refine_ls_extinction_coef        0.030(6) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          3437 
_refine_ls_number_parameters      191 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0880 
_refine_ls_R_factor_gt            0.0558 
_refine_ls_wR_factor_ref          0.1873 
_refine_ls_wR_factor_gt           0.1499 
_refine_ls_goodness_of_fit_ref    1.005 
_refine_ls_restrained_S_all       1.005 
_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 
Br1 Br 1.24672(5) 1.19751(6) 0.45613(5) 0.0760(3) Uani 1 1 d . . . 
C1 C 1.0257(5) 1.0733(5) 0.3205(4) 0.0542(9) Uani 1 1 d . . . 
O1 O 0.3167(4) 0.6895(4) -0.2108(3) 0.0627(7) Uani 1 1 d . . . 
C8 C 0.3896(4) 0.7118(4) 0.0267(4) 0.0455(8) Uani 1 1 d . . . 
O2 O 0.5666(4) 0.8496(4) -0.1920(3) 0.0709(8) Uani 1 1 d . . . 
C7 C 0.5271(5) 0.7981(5) 0.0135(4) 0.0475(8) Uani 1 1 d . . . 
C9 C 0.3699(4) 0.6869(4) 0.1556(4) 0.0466(8) Uani 1 1 d . . . 
C3 C 0.8298(5) 0.8910(5) 0.0785(4) 0.0516(9) Uani 1 1 d . . . 
H3A H 0.8073 0.8284 -0.0186 0.062 Uiso 1 1 calc R . . 
C18 C 0.1128(5) 0.6948(6) -0.1078(5) 0.0668(11) Uani 1 1 d . . . 
H18A H 0.1651 0.8128 -0.0628 0.100 Uiso 1 1 calc R . . 
H18B H 0.0575 0.6549 -0.0507 0.100 Uiso 1 1 calc R . . 
H18C H 0.0336 0.6558 -0.2046 0.100 Uiso 1 1 calc R . . 
C4 C 0.6995(5) 0.8938(4) 0.1202(4) 0.0478(8) Uani 1 1 d . . . 
C2 C 0.9913(5) 0.9784(5) 0.1772(5) 0.0560(9) Uani 1 1 d . . . 
H2A H 1.0767 0.9736 0.1475 0.067 Uiso 1 1 calc R . . 
C15 C 0.4808(5) 0.7862(5) -0.1365(4) 0.0561(10) Uani 1 1 d . . . 
C6 C 0.8987(5) 1.0813(6) 0.3636(5) 0.0660(12) Uani 1 1 d . . . 
H6A H 0.9227 1.1483 0.4597 0.079 Uiso 1 1 calc R . . 
C5 C 0.7373(5) 0.9914(5) 0.2660(4) 0.0595(10) Uani 1 1 d . . . 
H5A H 0.6526 0.9953 0.2971 0.071 Uiso 1 1 calc R . . 
C14 C 0.3809(5) 0.5554(5) 0.1779(5) 0.0589(10) Uani 1 1 d . . . 
H14A H 0.4010 0.4818 0.1111 0.071 Uiso 1 1 calc R . . 
C12 C 0.3315(6) 0.6374(7) 0.3964(5) 0.0768(15) Uani 1 1 d . . . 
H12A H 0.3174 0.6204 0.4765 0.092 Uiso 1 1 calc R . . 
C10 C 0.3378(5) 0.7946(6) 0.2552(5) 0.0626(11) Uani 1 1 d . . . 
H10A H 0.3275 0.8828 0.2406 0.075 Uiso 1 1 calc R . . 
C16 C 0.2445(5) 0.6325(5) -0.1161(4) 0.0525(9) Uani 1 1 d . . . 
C13 C 0.3625(6) 0.5311(6) 0.2980(5) 0.0695(12) Uani 1 1 d . . . 
H13A H 0.3713 0.4420 0.3120 0.083 Uiso 1 1 calc R . . 
C11 C 0.3211(6) 0.7711(7) 0.3756(5) 0.0730(14) Uani 1 1 d . . . 
H11A H 0.3028 0.8454 0.4435 0.088 Uiso 1 1 calc R . . 
C17 C 0.1691(6) 0.4471(5) -0.1851(5) 0.0724(12) Uani 1 1 d . . . 
H17A H 0.2545 0.4126 -0.1889 0.109 Uiso 1 1 calc R . . 
H17B H 0.0895 0.4051 -0.2824 0.109 Uiso 1 1 calc R . . 
H17C H 0.1153 0.4057 -0.1278 0.109 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 
Br1 C1 1.884(4) . ? 
C1 C6 1.379(6) . ? 
C1 C2 1.377(6) . ? 
O1 C15 1.350(5) . ? 
O1 C16 1.461(5) . ? 
C8 C7 1.336(5) . ? 
C8 C9 1.477(5) . ? 
C8 C16 1.501(5) . ? 
O2 C15 1.207(5) . ? 
C7 C4 1.472(5) . ? 
C7 C15 1.475(5) . ? 
C9 C14 1.374(6) . ? 
C9 C10 1.387(5) . ? 
C3 C2 1.375(6) . ? 
C3 C4 1.390(5) . ? 
C18 C16 1.538(6) . ? 
C4 C5 1.397(5) . ? 
C6 C5 1.371(6) . ? 
C14 C13 1.382(6) . ? 
C12 C13 1.366(7) . ? 
C12 C11 1.386(8) . ? 
C10 C11 1.377(6) . ? 
C16 C17 1.510(6) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C6 C1 C2 119.9(4) . . ? 
C6 C1 Br1 120.1(3) . . ? 
C2 C1 Br1 120.0(3) . . ? 
C15 O1 C16 109.9(3) . . ? 
C7 C8 C9 128.9(3) . . ? 
C7 C8 C16 110.0(3) . . ? 
C9 C8 C16 121.1(3) . . ? 
C8 C7 C4 130.7(3) . . ? 
C8 C7 C15 107.9(4) . . ? 
C4 C7 C15 121.4(3) . . ? 
C14 C9 C10 118.8(4) . . ? 
C14 C9 C8 120.6(3) . . ? 
C10 C9 C8 120.6(4) . . ? 
C2 C3 C4 121.5(4) . . ? 
C3 C4 C5 118.0(4) . . ? 
C3 C4 C7 120.9(3) . . ? 
C5 C4 C7 121.1(3) . . ? 
C3 C2 C1 119.5(4) . . ? 
O2 C15 O1 121.9(4) . . ? 
O2 C15 C7 129.2(4) . . ? 
O1 C15 C7 108.9(3) . . ? 
C5 C6 C1 120.7(4) . . ? 
C6 C5 C4 120.4(4) . . ? 
C9 C14 C13 121.0(4) . . ? 
C13 C12 C11 119.4(4) . . ? 
C11 C10 C9 120.1(5) . . ? 
O1 C16 C8 103.3(3) . . ? 
O1 C16 C17 107.6(3) . . ? 
C8 C16 C17 113.8(4) . . ? 
O1 C16 C18 106.6(3) . . ? 
C8 C16 C18 113.1(3) . . ? 
C17 C16 C18 111.7(4) . . ? 
C12 C13 C14 120.2(5) . . ? 
C10 C11 C12 120.5(4) . . ? 
 
_diffrn_measured_fraction_theta_max    0.981 
_diffrn_reflns_theta_full              27.47 
_diffrn_measured_fraction_theta_full   0.981 
_refine_diff_density_max    0.569 
_refine_diff_density_min   -0.642 
_refine_diff_density_rms    0.202 
