 
data_PO19060O_002
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C34 H24 O4' 
_chemical_formula_weight          496.53

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0034   0.0017
 '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'   0.0116   0.0065
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    9.3460(19)
_cell_length_b                    10.173(2)
_cell_length_c                    14.036(3)
_cell_angle_alpha                 95.94(3)
_cell_angle_beta                  102.85(3)
_cell_angle_gamma                 94.02(3)
_cell_volume                      1288.1(5)
_cell_formula_units_Z             2
_cell_measurement_temperature     223(2)
_cell_measurement_reflns_used     21679
_cell_measurement_theta_min       0.418
_cell_measurement_theta_max       33.575
 
_exptl_crystal_description        'plate'
_exptl_crystal_colour             'green'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.280          
_exptl_crystal_F_000              520
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.082
_exptl_crystal_size_mid           0.032
_exptl_crystal_size_min           0.017
_exptl_absorpt_coefficient_mu     0.087
_shelx_estimated_absorpt_T_min    0.993
_shelx_estimated_absorpt_T_max    0.999
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.917
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    'HKL3000sm Scalepack'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       223(2)
_diffrn_radiation_wavelength      0.730
_diffrn_radiation_type            synchrotron
_diffrn_source                    'PLSII 2D bending magnet'
_diffrn_measurement_device_type   'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method        'omega scan'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             13532
_diffrn_reflns_av_unetI/netI      0.0440
_diffrn_reflns_av_R_equivalents   0.0292
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.540
_diffrn_reflns_theta_max          29.999
_diffrn_reflns_theta_full         25.976
_diffrn_measured_fraction_theta_max   0.988
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.988
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.988
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              6851
_reflns_number_gt                 3871
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'PAL BL2D-SMDC Program'
_computing_cell_refinement        'HKL3000sm'
_computing_data_reduction         'HKL3000sm'
_computing_structure_solution     SHELXS
_computing_structure_refinement   SHELXL
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1946P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          6851
_refine_ls_number_parameters      344
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1267
_refine_ls_R_factor_gt            0.0863
_refine_ls_wR_factor_ref          0.3119
_refine_ls_wR_factor_gt           0.2796
_refine_ls_goodness_of_fit_ref    1.107
_refine_ls_restrained_S_all       1.107
_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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.6713(3) 0.4473(2) 0.31923(16) 0.0528(5) Uani 1 1 d . . . . .
C2 C 0.6269(3) 0.3392(3) 0.24472(17) 0.0560(6) Uani 1 1 d . . . . .
C3 C 0.6263(3) 0.2241(3) 0.29122(17) 0.0566(6) Uani 1 1 d . . . . .
C4 C 0.5957(3) 0.0950(3) 0.24268(19) 0.0665(7) Uani 1 1 d . . . . .
H4 H 0.574603 0.088123 0.173576 0.080 Uiso 1 1 calc R U . . .
C5 C 0.5918(4) -0.0243(3) 0.2816(2) 0.0726(8) Uani 1 1 d . . . . .
H5 H 0.570839 -0.100896 0.235433 0.087 Uiso 1 1 calc R U . . .
C6 C 0.6147(3) -0.0463(3) 0.3801(2) 0.0723(7) Uani 1 1 d . . . . .
H6 H 0.599330 -0.135582 0.390422 0.087 Uiso 1 1 calc R U . . .
C7 C 0.6558(3) 0.0416(3) 0.4638(2) 0.0680(7) Uani 1 1 d . . . . .
H7 H 0.668109 0.004556 0.523386 0.082 Uiso 1 1 calc R U . . .
C8 C 0.6819(3) 0.1787(3) 0.47217(18) 0.0610(6) Uani 1 1 d . . . . .
H8 H 0.712470 0.221222 0.537071 0.073 Uiso 1 1 calc R U . . .
C9 C 0.6699(3) 0.2630(3) 0.39960(16) 0.0544(6) Uani 1 1 d . . . . .
C10 C 0.6974(3) 0.4034(2) 0.41316(16) 0.0532(6) Uani 1 1 d . . . . .
C11 C 0.7442(3) 0.4984(3) 0.50069(16) 0.0538(6) Uani 1 1 d . . . . .
C12 C 0.7773(3) 0.4567(3) 0.60173(16) 0.0558(6) Uani 1 1 d . . . . .
C13 C 0.6648(3) 0.4272(3) 0.64863(19) 0.0658(7) Uani 1 1 d . . . . .
H13 H 0.566479 0.434978 0.616964 0.079 Uiso 1 1 calc R U . . .
C14 C 0.6965(4) 0.3862(3) 0.7422(2) 0.0752(8) Uani 1 1 d . . . . .
H14 H 0.619767 0.366568 0.773447 0.090 Uiso 1 1 calc R U . . .
C15 C 0.8394(4) 0.3745(4) 0.7885(2) 0.0801(9) Uani 1 1 d . . . . .
H15 H 0.860826 0.346901 0.851601 0.096 Uiso 1 1 calc R U . . .
C16 C 0.9525(4) 0.4033(4) 0.7425(2) 0.0890(10) Uani 1 1 d . . . . .
H16 H 1.050641 0.395035 0.774222 0.107 Uiso 1 1 calc R U . . .
C17 C 0.9205(3) 0.4446(3) 0.64926(19) 0.0700(7) Uani 1 1 d . . . . .
H17 H 0.997535 0.464363 0.618369 0.084 Uiso 1 1 calc R U . . .
C18 C 0.7678(3) 0.6270(3) 0.48804(16) 0.0553(6) Uani 1 1 d . . . . .
C19 C 0.8183(3) 0.7412(3) 0.56377(16) 0.0569(6) Uani 1 1 d . . . . .
C20 C 0.7481(3) 0.7683(3) 0.64094(18) 0.0632(7) Uani 1 1 d . . . . .
H20 H 0.667345 0.710922 0.645754 0.076 Uiso 1 1 calc R U . . .
C21 C 0.7959(4) 0.8777(3) 0.70975(19) 0.0738(8) Uani 1 1 d . . . . .
H21 H 0.748182 0.895202 0.761342 0.089 Uiso 1 1 calc R U . . .
C22 C 0.9139(4) 0.9615(3) 0.7027(2) 0.0787(9) Uani 1 1 d . . . . .
H22 H 0.946950 1.036356 0.749710 0.094 Uiso 1 1 calc R U . . .
C23 C 0.9843(4) 0.9362(3) 0.6268(2) 0.0768(8) Uani 1 1 d . . . . .
H23 H 1.065605 0.993623 0.622904 0.092 Uiso 1 1 calc R U . . .
C24 C 0.9362(3) 0.8277(3) 0.55699(19) 0.0668(7) Uani 1 1 d . . . . .
H24 H 0.983054 0.812102 0.504739 0.080 Uiso 1 1 calc R U . . .
O25 O 0.7459(2) 0.66783(17) 0.39451(11) 0.0585(5) Uani 1 1 d . . . . .
C26 C 0.6938(3) 0.5855(2) 0.30820(16) 0.0543(6) Uani 1 1 d . . . . .
O27 O 0.6734(2) 0.63784(18) 0.23293(12) 0.0658(5) Uani 1 1 d . . . . .
C28 C 0.5895(3) 0.3506(3) 0.13492(17) 0.0600(6) Uani 1 1 d . . . . .
H28 H 0.614162 0.444721 0.127757 0.072 Uiso 1 1 calc R U . . .
C29 C 0.6827(3) 0.2685(3) 0.07879(17) 0.0610(6) Uani 1 1 d . . . . .
C30 C 0.8284(4) 0.2611(3) 0.1199(2) 0.0733(8) Uani 1 1 d . . . . .
H30 H 0.869445 0.304705 0.183537 0.088 Uiso 1 1 calc R U . . .
C31 C 0.9182(4) 0.1903(4) 0.0699(2) 0.0793(9) Uani 1 1 d . . . . .
H31 H 1.018453 0.187607 0.099452 0.095 Uiso 1 1 calc R U . . .
C32 C 0.8596(4) 0.1251(4) -0.0221(2) 0.0827(9) Uani 1 1 d . . . . .
H32 H 0.918584 0.075986 -0.055832 0.099 Uiso 1 1 calc R U . . .
C33 C 0.7142(5) 0.1321(4) -0.0646(2) 0.0965(11) Uani 1 1 d . . . . .
H33 H 0.673612 0.088155 -0.128223 0.116 Uiso 1 1 calc R U . . .
C34 C 0.6249(4) 0.2039(4) -0.0148(2) 0.0845(10) Uani 1 1 d . . . . .
H34 H 0.525276 0.208132 -0.045131 0.101 Uiso 1 1 calc R U . . .
C35 C 0.4251(3) 0.3202(3) 0.09257(18) 0.0645(7) Uani 1 1 d . . . . .
O36 O 0.3514(3) 0.2247(3) 0.1042(2) 0.0967(8) Uani 1 1 d . . . . .
O37 O 0.3684(2) 0.4133(2) 0.04107(16) 0.0832(6) Uani 1 1 d . . . . .
C38 C 0.2129(4) 0.3917(5) -0.0049(3) 0.1010(12) Uani 1 1 d . . . . .
H38A H 0.184473 0.463856 -0.043013 0.152 Uiso 1 1 calc R U . . .
H38B H 0.156962 0.388313 0.045420 0.152 Uiso 1 1 calc R U . . .
H38C H 0.192917 0.308399 -0.048060 0.152 Uiso 1 1 calc R U . . .
 
 
_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 1.407(3) . ?
C1 C10 1.411(3) . ?
C1 C26 1.436(3) . ?
C2 C3 1.398(4) . ?
C2 C28 1.521(3) . ?
C3 C4 1.395(4) . ?
C3 C9 1.488(3) . ?
C4 C5 1.383(4) . ?
C4 H4 0.9400 . ?
C5 C6 1.396(4) . ?
C5 H5 0.9400 . ?
C6 C7 1.364(4) . ?
C6 H6 0.9400 . ?
C7 C8 1.388(4) . ?
C7 H7 0.9400 . ?
C8 C9 1.389(3) . ?
C8 H8 0.9400 . ?
C9 C10 1.419(4) . ?
C10 C11 1.446(3) . ?
C11 C18 1.348(4) . ?
C11 C12 1.495(3) . ?
C12 C17 1.376(4) . ?
C12 C13 1.391(4) . ?
C13 C14 1.395(4) . ?
C13 H13 0.9400 . ?
C14 C15 1.368(4) . ?
C14 H14 0.9400 . ?
C15 C16 1.386(5) . ?
C15 H15 0.9400 . ?
C16 C17 1.391(4) . ?
C16 H16 0.9400 . ?
C17 H17 0.9400 . ?
C18 O25 1.394(3) . ?
C18 C19 1.465(3) . ?
C19 C24 1.387(4) . ?
C19 C20 1.400(3) . ?
C20 C21 1.374(4) . ?
C20 H20 0.9400 . ?
C21 C22 1.373(5) . ?
C21 H21 0.9400 . ?
C22 C23 1.383(5) . ?
C22 H22 0.9400 . ?
C23 C24 1.376(4) . ?
C23 H23 0.9400 . ?
C24 H24 0.9400 . ?
O25 C26 1.370(3) . ?
C26 O27 1.215(3) . ?
C28 C35 1.516(4) . ?
C28 C29 1.532(4) . ?
C28 H28 0.9900 . ?
C29 C30 1.367(4) . ?
C29 C34 1.380(4) . ?
C30 C31 1.400(4) . ?
C30 H30 0.9400 . ?
C31 C32 1.365(4) . ?
C31 H31 0.9400 . ?
C32 C33 1.368(5) . ?
C32 H32 0.9400 . ?
C33 C34 1.399(5) . ?
C33 H33 0.9400 . ?
C34 H34 0.9400 . ?
C35 O36 1.198(4) . ?
C35 O37 1.319(3) . ?
O37 C38 1.444(4) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
 
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 C10 110.7(2) . . ?
C2 C1 C26 128.0(2) . . ?
C10 C1 C26 121.2(2) . . ?
C3 C2 C1 107.1(2) . . ?
C3 C2 C28 128.1(2) . . ?
C1 C2 C28 124.8(2) . . ?
C4 C3 C2 124.9(2) . . ?
C4 C3 C9 126.5(2) . . ?
C2 C3 C9 108.5(2) . . ?
C5 C4 C3 129.3(3) . . ?
C5 C4 H4 115.3 . . ?
C3 C4 H4 115.3 . . ?
C4 C5 C6 128.8(3) . . ?
C4 C5 H5 115.6 . . ?
C6 C5 H5 115.6 . . ?
C7 C6 C5 130.0(3) . . ?
C7 C6 H6 115.0 . . ?
C5 C6 H6 115.0 . . ?
C6 C7 C8 128.3(3) . . ?
C6 C7 H7 115.8 . . ?
C8 C7 H7 115.8 . . ?
C7 C8 C9 130.0(3) . . ?
C7 C8 H8 115.0 . . ?
C9 C8 H8 115.0 . . ?
C8 C9 C10 127.3(2) . . ?
C8 C9 C3 126.9(2) . . ?
C10 C9 C3 105.8(2) . . ?
C1 C10 C9 107.8(2) . . ?
C1 C10 C11 120.1(2) . . ?
C9 C10 C11 132.1(2) . . ?
C18 C11 C10 117.4(2) . . ?
C18 C11 C12 120.3(2) . . ?
C10 C11 C12 122.2(2) . . ?
C17 C12 C13 118.8(2) . . ?
C17 C12 C11 120.2(2) . . ?
C13 C12 C11 120.9(2) . . ?
C12 C13 C14 120.6(3) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C15 C14 C13 119.9(3) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.1(3) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C17 119.8(3) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C12 C17 C16 120.8(3) . . ?
C12 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C11 C18 O25 121.6(2) . . ?
C11 C18 C19 128.1(2) . . ?
O25 C18 C19 110.3(2) . . ?
C24 C19 C20 118.9(2) . . ?
C24 C19 C18 119.0(2) . . ?
C20 C19 C18 122.0(3) . . ?
C21 C20 C19 120.7(3) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C22 C21 C20 119.6(3) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C21 C22 C23 120.4(3) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C24 C23 C22 120.4(3) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C19 119.9(3) . . ?
C23 C24 H24 120.0 . . ?
C19 C24 H24 120.0 . . ?
C26 O25 C18 124.63(19) . . ?
O27 C26 O25 116.5(2) . . ?
O27 C26 C1 128.6(2) . . ?
O25 C26 C1 114.93(19) . . ?
C35 C28 C2 110.5(2) . . ?
C35 C28 C29 113.2(2) . . ?
C2 C28 C29 112.7(2) . . ?
C35 C28 H28 106.7 . . ?
C2 C28 H28 106.7 . . ?
C29 C28 H28 106.7 . . ?
C30 C29 C34 118.1(3) . . ?
C30 C29 C28 120.1(2) . . ?
C34 C29 C28 121.8(3) . . ?
C29 C30 C31 121.8(3) . . ?
C29 C30 H30 119.1 . . ?
C31 C30 H30 119.1 . . ?
C32 C31 C30 119.7(3) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
C31 C32 C33 119.3(3) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
C32 C33 C34 120.9(3) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
C29 C34 C33 120.2(3) . . ?
C29 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
O36 C35 O37 122.2(3) . . ?
O36 C35 C28 125.4(3) . . ?
O37 C35 C28 112.4(3) . . ?
C35 O37 C38 116.6(3) . . ?
O37 C38 H38A 109.5 . . ?
O37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
 
_refine_diff_density_max    0.337
_refine_diff_density_min   -0.368
_refine_diff_density_rms    0.064





















