 
data_BiAz1_a
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C20 H14'
_chemical_formula_sum
 'C20 H14' 
_chemical_formula_weight          254.31

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    14.0565(7)
_cell_length_b                    5.9201(3)
_cell_length_c                    7.8474(4)
_cell_angle_alpha                 90
_cell_angle_beta                  92.837(3)
_cell_angle_gamma                 90
_cell_volume                      652.23(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     296
_cell_measurement_reflns_used     3891
_cell_measurement_theta_min       3.15
_cell_measurement_theta_max       67.87
 
_exptl_crystal_description        'Platelet'
_exptl_crystal_colour             'Blue'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.295          
_exptl_crystal_F_000              268
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.130
_exptl_crystal_size_mid           0.090
_exptl_crystal_size_min           0.030
_exptl_absorpt_coefficient_mu     0.554
_shelx_estimated_absorpt_T_min    0.931
_shelx_estimated_absorpt_T_max    0.984
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.7333
_exptl_absorpt_correction_T_max   1.0000
_exptl_absorpt_process_details    '(ABSCOR; Higashi, 1995)'
_exptl_absorpt_special_details    
; 
 Higashi, T. (1995). Program for Absorption Correction.
 Rigaku Corporation, Tokyo, Japan. 
; 
_diffrn_ambient_temperature       296
_diffrn_radiation_wavelength      1.54187
_diffrn_radiation_type            CuK\a
_diffrn_source                    'rotating anode'
_diffrn_measurement_device_type   'Rigaku RAXIS-RAPID'
_diffrn_measurement_method        ω
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             11264
_diffrn_reflns_av_unetI/netI      0.0740
_diffrn_reflns_av_R_equivalents   0.0983
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -7
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_theta_min          3.148
_diffrn_reflns_theta_max          68.222
_diffrn_reflns_theta_full         67.687
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              1191
_reflns_number_gt                 413
_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        'PROCESS-AUTO (Rigaku, 1998)'
_computing_cell_refinement        'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction         'PROCESS-AUTO (Rigaku, 1998)'  
_computing_structure_solution     'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material   'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_publ_section_references	
;
Wakita, K. (2001). Yadokari-XG. Software for Crystal Structure Analyses.
Release of Software (Yadokari-XG 2009) for Crystal Structure Analyses,
Kabuto, C., Akine, S., Nemoto, T. and Kwon, E. (2009). J. Cryst. Soc. Jpn.,
51, 218-224.
;
_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
'w=1/[σ²(Fo²)+(0.1980P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          1191
_refine_ls_number_parameters      181
_refine_ls_number_restraints      138
_refine_ls_R_factor_all           0.1901
_refine_ls_R_factor_gt            0.0958
_refine_ls_wR_factor_ref          0.3442
_refine_ls_wR_factor_gt           0.2527
_refine_ls_goodness_of_fit_ref    0.905
_refine_ls_restrained_S_all       0.867
_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
C1A C 0.1485(17) 0.669(4) 0.740(3) 0.076(3) Uani 0.5 1 d . U P A -1
H1A H 0.1343 0.7926 0.8068 0.091 Uiso 0.5 1 calc R U P A -1
C2A C 0.0862(15) 0.489(3) 0.689(3) 0.079(3) Uani 0.5 1 d . U P A -1
H2A H 0.0220 0.4904 0.7126 0.095 Uiso 0.5 1 calc R U P A -1
C3A C 0.1268(19) 0.308(3) 0.601(3) 0.076(3) Uani 0.5 1 d . U P A -1
H3A H 0.0996 0.1723 0.5643 0.091 Uiso 0.5 1 calc R U P A -1
C4A C 0.2937(10) 0.274(2) 0.5047(13) 0.076(3) Uani 0.5 1 d . U P A -1
H4A H 0.2716 0.1346 0.4641 0.091 Uiso 0.5 1 calc R U P A -1
C5A C 0.382(2) 0.308(5) 0.476(4) 0.071(3) Uani 0.5 1 d . U P A -1
H5A H 0.4099 0.1950 0.4124 0.085 Uiso 0.5 1 calc R U P A -1
C6A C 0.445(3) 0.493(8) 0.525(7) 0.070(3) Uani 0.5 1 d . U P A -1
C7A C 0.410(3) 0.692(5) 0.607(3) 0.074(3) Uani 0.5 1 d . U P A -1
H7A H 0.4531 0.8116 0.6125 0.089 Uiso 0.5 1 calc R U P A -1
C8A C 0.3246(9) 0.738(2) 0.6774(14) 0.075(2) Uani 0.5 1 d . U P A -1
H8A H 0.3232 0.8673 0.7442 0.090 Uiso 0.5 1 calc R U P A -1
C9A C 0.2412(9) 0.6178(19) 0.6629(14) 0.076(2) Uani 0.5 1 d . U P A -1
C10A C 0.2248(9) 0.3950(19) 0.5819(13) 0.075(2) Uani 0.5 1 d . U P A -1
C11A C 0.606(2) 0.665(5) 0.510(4) 0.073(3) Uani 0.5 1 d . U P A -1
H11A H 0.5913 0.7990 0.5657 0.088 Uiso 0.5 1 calc R U P A -1
C12A C 0.544(3) 0.495(9) 0.476(7) 0.070(3) Uani 0.5 1 d . U P A -1
C13A C 0.586(3) 0.332(5) 0.375(3) 0.074(3) Uani 0.5 1 d . U P A -1
H13A H 0.5549 0.2091 0.3225 0.089 Uiso 0.5 1 calc R U P A -1
C14A C 0.7504(10) 0.264(2) 0.2878(13) 0.078(2) Uani 0.5 1 d . U P A -1
H14A H 0.7258 0.1357 0.2333 0.093 Uiso 0.5 1 calc R U P A -1
C15A C 0.8391(19) 0.287(4) 0.275(3) 0.077(3) Uani 0.5 1 d . U P A -1
H15A H 0.8683 0.1662 0.2222 0.092 Uiso 0.5 1 calc R U P A -1
C16A C 0.8989(15) 0.456(3) 0.323(3) 0.083(4) Uani 0.5 1 d . U P A -1
H16A H 0.9624 0.4463 0.2956 0.100 Uiso 0.5 1 calc R U P A -1
C17A C 0.869(2) 0.642(3) 0.413(4) 0.080(3) Uani 0.5 1 d . U P A -1
H17A H 0.9205 0.7340 0.4459 0.096 Uiso 0.5 1 calc R U P A -1
C18A C 0.7834(9) 0.728(2) 0.4669(14) 0.077(2) Uani 0.5 1 d . U P A -1
H18A H 0.7831 0.8708 0.5168 0.093 Uiso 0.5 1 calc R U P A -1
C19A C 0.6992(9) 0.6098(19) 0.4487(14) 0.074(2) Uani 0.5 1 d . U P A -1
C20A C 0.6827(9) 0.3892(19) 0.3659(13) 0.075(2) Uani 0.5 1 d . U P A -1
 
 
_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
C1A C2A 1.42(2) . ?
C1A C9A 1.49(3) . ?
C1A H1A 0.9300 . ?
C2A C3A 1.41(3) . ?
C2A H2A 0.9300 . ?
C3A C10A 1.48(3) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.29(3) . ?
C4A C10A 1.370(17) . ?
C4A H4A 0.9300 . ?
C5A C6A 1.45(4) . ?
C5A H5A 0.9300 . ?
C6A C7A 1.44(6) . ?
C6A C12A 1.466(9) . ?
C7A C8A 1.38(4) . ?
C7A H7A 0.9300 . ?
C8A C9A 1.370(16) . ?
C8A H8A 0.9300 . ?
C9A C10A 1.477(17) . ?
C11A C12A 1.35(4) . ?
C11A C19A 1.46(3) . ?
C11A H11A 0.9300 . ?
C12A C13A 1.39(6) . ?
C13A C20A 1.41(4) . ?
C13A H13A 0.9300 . ?
C14A C15A 1.26(3) . ?
C14A C20A 1.374(16) . ?
C14A H14A 0.9300 . ?
C15A C16A 1.35(2) . ?
C15A H15A 0.9300 . ?
C16A C17A 1.38(3) . ?
C16A H16A 0.9300 . ?
C17A C18A 1.40(3) . ?
C17A H17A 0.9300 . ?
C18A C19A 1.378(15) . ?
C18A H18A 0.9300 . ?
C19A C20A 1.472(17) . ?
 
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
C2A C1A C9A 105.8(17) . . ?
C2A C1A H1A 127.1 . . ?
C9A C1A H1A 127.1 . . ?
C3A C2A C1A 116.6(16) . . ?
C3A C2A H2A 121.7 . . ?
C1A C2A H2A 121.7 . . ?
C2A C3A C10A 100.8(14) . . ?
C2A C3A H3A 129.6 . . ?
C10A C3A H3A 129.6 . . ?
C5A C4A C10A 134.7(19) . . ?
C5A C4A H4A 112.6 . . ?
C10A C4A H4A 112.6 . . ?
C4A C5A C6A 131(3) . . ?
C4A C5A H5A 114.7 . . ?
C6A C5A H5A 114.7 . . ?
C7A C6A C5A 122(3) . . ?
C7A C6A C12A 118(2) . . ?
C5A C6A C12A 121(2) . . ?
C8A C7A C6A 132(3) . . ?
C8A C7A H7A 114.2 . . ?
C6A C7A H7A 114.2 . . ?
C9A C8A C7A 129(2) . . ?
C9A C8A H8A 115.6 . . ?
C7A C8A H8A 115.6 . . ?
C8A C9A C10A 127.8(14) . . ?
C8A C9A C1A 128.4(16) . . ?
C10A C9A C1A 103.5(11) . . ?
C4A C10A C9A 124.0(14) . . ?
C4A C10A C3A 122.8(15) . . ?
C9A C10A C3A 113.1(13) . . ?
C12A C11A C19A 110(2) . . ?
C12A C11A H11A 124.9 . . ?
C19A C11A H11A 124.9 . . ?
C11A C12A C13A 110(3) . . ?
C11A C12A C6A 124(2) . . ?
C13A C12A C6A 125(2) . . ?
C12A C13A C20A 107(3) . . ?
C12A C13A H13A 126.5 . . ?
C20A C13A H13A 126.5 . . ?
C15A C14A C20A 133.3(19) . . ?
C15A C14A H14A 113.3 . . ?
C20A C14A H14A 113.3 . . ?
C14A C15A C16A 131(2) . . ?
C14A C15A H15A 114.3 . . ?
C16A C15A H15A 114.3 . . ?
C15A C16A C17A 122.4(18) . . ?
C15A C16A H16A 118.8 . . ?
C17A C16A H16A 118.8 . . ?
C16A C17A C18A 137(2) . . ?
C16A C17A H17A 111.4 . . ?
C18A C17A H17A 111.4 . . ?
C19A C18A C17A 122.2(17) . . ?
C19A C18A H18A 118.9 . . ?
C17A C18A H18A 118.9 . . ?
C18A C19A C11A 129.2(16) . . ?
C18A C19A C20A 127.8(14) . . ?
C11A C19A C20A 102.9(12) . . ?
C14A C20A C13A 125.8(19) . . ?
C14A C20A C19A 125.3(14) . . ?
C13A C20A C19A 108.8(16) . . ?
 
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
C9A C1A C2A C3A 6(2) . . . . ?
C1A C2A C3A C10A -5(2) . . . . ?
C10A C4A C5A C6A 4(4) . . . . ?
C4A C5A C6A C7A -7(6) . . . . ?
C4A C5A C6A C12A -180(2) . . . . ?
C5A C6A C7A C8A 12(6) . . . . ?
C12A C6A C7A C8A -175.0(19) . . . . ?
C6A C7A C8A C9A -13(4) . . . . ?
C7A C8A C9A C10A 7(2) . . . . ?
C7A C8A C9A C1A -179.7(18) . . . . ?
C2A C1A C9A C8A -178.5(13) . . . . ?
C2A C1A C9A C10A -4.1(15) . . . . ?
C5A C4A C10A C9A -2(3) . . . . ?
C5A C4A C10A C3A -179(2) . . . . ?
C8A C9A C10A C4A -0.9(17) . . . . ?
C1A C9A C10A C4A -175.4(13) . . . . ?
C8A C9A C10A C3A 175.8(13) . . . . ?
C1A C9A C10A C3A 1.4(15) . . . . ?
C2A C3A C10A C4A 178.7(12) . . . . ?
C2A C3A C10A C9A 1.9(17) . . . . ?
C19A C11A C12A C13A -7(4) . . . . ?
C19A C11A C12A C6A 178.1(15) . . . . ?
C7A C6A C12A C11A 4(2) . . . . ?
C5A C6A C12A C11A 177(5) . . . . ?
C7A C6A C12A C13A -170(6) . . . . ?
C5A C6A C12A C13A 3(2) . . . . ?
C11A C12A C13A C20A 9(4) . . . . ?
C6A C12A C13A C20A -176.6(12) . . . . ?
C20A C14A C15A C16A -6(3) . . . . ?
C14A C15A C16A C17A 4(3) . . . . ?
C15A C16A C17A C18A -6(3) . . . . ?
C16A C17A C18A C19A 7(3) . . . . ?
C17A C18A C19A C11A 174(2) . . . . ?
C17A C18A C19A C20A -4(2) . . . . ?
C12A C11A C19A C18A -175(3) . . . . ?
C12A C11A C19A C20A 3(3) . . . . ?
C15A C14A C20A C13A -176.9(19) . . . . ?
C15A C14A C20A C19A 6(2) . . . . ?
C12A C13A C20A C14A 175(3) . . . . ?
C12A C13A C20A C19A -7(3) . . . . ?
C18A C19A C20A C14A -1.5(17) . . . . ?
C11A C19A C20A C14A -179.6(16) . . . . ?
C18A C19A C20A C13A -179.3(13) . . . . ?
C11A C19A C20A C13A 2.6(17) . . . . ?
 
_refine_diff_density_max    0.195
_refine_diff_density_min   -0.210
_refine_diff_density_rms    0.058

# start Validation Reply Form
_vrf_PLAT026_BiAz1_a
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..
RESPONSE: This structure was disordered by a pseudo inversion center and 
with low diffracting power because of their thin shape. 
Consequently, a number of reflections were missing especially 
in the range of 0.91-0.77 angstrom resolution.
;
_vrf_PLAT088_BiAz1_a
;
PROBLEM: Poor Data / Parameter Ratio ....................
RESPONSE: This structure was disordered by a pseudo inversion center and 
with low diffracting power because of their thin shape. 
Consequently, a number of reflections were missing especially 
in the range of 0.91-0.77 angstrom resolution.
;
# end Validation Reply Form



