 
data_180625_kazu_1_rt_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'   0.0033   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'
 
_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                    13.5349(7)
_cell_length_b                    6.0042(3)
_cell_length_c                    8.1543(4)
_cell_angle_alpha                 90
_cell_angle_beta                  94.232(4)
_cell_angle_gamma                 90
_cell_volume                      660.86(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     293
_cell_measurement_reflns_used     3976
_cell_measurement_theta_min       2.8870
_cell_measurement_theta_max       30.4250
 
_exptl_crystal_description        'Prism'
_exptl_crystal_colour             'Colorless'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.278          
_exptl_crystal_F_000              268
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.150
_exptl_crystal_size_mid           0.100
_exptl_crystal_size_min           0.050
_exptl_absorpt_coefficient_mu     0.072
_shelx_estimated_absorpt_T_min    0.989
_shelx_estimated_absorpt_T_max    0.996
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.68727
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_process_details    
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min           0.832
_oxdiff_exptl_absorpt_empirical_full_max           1.214
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;

_diffrn_ambient_temperature       293
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'Rotating Anode'
_diffrn_measurement_device_type   'Rigaku Saturn 70 CCD area detector'
_diffrn_measurement_method        'ω'
_diffrn_detector_area_resol_mean  28.5714
_diffrn_reflns_number             8657
_diffrn_reflns_av_unetI/netI      0.0237
_diffrn_reflns_av_R_equivalents   0.0400
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -7
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          3.714
_diffrn_reflns_theta_max          27.495
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.993
_diffrn_measured_fraction_theta_full  0.991
_diffrn_reflns_Laue_measured_fraction_max    0.993
_diffrn_reflns_Laue_measured_fraction_full   0.991
_diffrn_reflns_point_group_measured_fraction_max   0.993
_diffrn_reflns_point_group_measured_fraction_full  0.991
_reflns_number_total              1514
_reflns_number_gt                 1117
_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        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction         'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution     'SHELXT (Sheldrick, 2015)'
_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           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0825P)²+0.0909P] 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          1514
_refine_ls_number_parameters      91
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0712
_refine_ls_R_factor_gt            0.0527
_refine_ls_wR_factor_ref          0.1550
_refine_ls_wR_factor_gt           0.1404
_refine_ls_goodness_of_fit_ref    1.080
_refine_ls_restrained_S_all       1.080
_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 0.55245(9) 0.5209(2) 0.53072(15) 0.0349(4) Uani 1 1 d . . . . .
C2 C 0.60645(10) 0.3700(2) 0.62854(16) 0.0376(4) Uani 1 1 d . . . . .
H2 H 0.5762 0.2383 0.6578 0.045 Uiso 1 1 calc R U . . .
C3 C 0.70653(10) 0.4085(2) 0.68604(15) 0.0364(4) Uani 1 1 d . . . . .
C4 C 0.76207(11) 0.2529(2) 0.78620(17) 0.0436(4) Uani 1 1 d . . . . .
H4 H 0.7328 0.1199 0.8153 0.052 Uiso 1 1 calc R U . . .
C5 C 0.85821(11) 0.2964(3) 0.84052(18) 0.0506(4) Uani 1 1 d . . . . .
H5 H 0.8937 0.1926 0.9058 0.061 Uiso 1 1 calc R U . . .
C6 C 0.90370(11) 0.4972(3) 0.7982(2) 0.0526(4) Uani 1 1 d . . . . .
H6 H 0.9689 0.5261 0.8364 0.063 Uiso 1 1 calc R U . . .
C7 C 0.85232(11) 0.6499(3) 0.70132(19) 0.0482(4) Uani 1 1 d . . . . .
H7 H 0.8833 0.7812 0.6729 0.058 Uiso 1 1 calc R U . . .
C8 C 0.75272(10) 0.6108(2) 0.64362(16) 0.0378(4) Uani 1 1 d . . . . .
C9 C 0.69672(11) 0.7650(2) 0.54395(17) 0.0427(4) Uani 1 1 d . . . . .
H9 H 0.7259 0.8980 0.5146 0.051 Uiso 1 1 calc R U . . .
C10 C 0.60091(10) 0.7225(2) 0.49008(17) 0.0424(4) Uani 1 1 d . . . . .
H10 H 0.5661 0.8277 0.4251 0.051 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 1.3805(19) . ?
C1 C10 1.4272(19) . ?
C1 C1 1.492(2) 3_666 ?
C2 C3 1.4194(19) . ?
C2 H2 0.9300 . ?
C3 C4 1.4192(19) . ?
C3 C8 1.421(2) . ?
C4 C5 1.368(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.408(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.366(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.4142(19) . ?
C7 H7 0.9300 . ?
C8 C9 1.4143(19) . ?
C9 C10 1.3622(19) . ?
C9 H9 0.9300 . ?
C10 H10 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
C2 C1 C10 117.27(12) . . ?
C2 C1 C1 122.26(15) . 3_666 ?
C10 C1 C1 120.47(15) . 3_666 ?
C1 C2 C3 122.38(12) . . ?
C1 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
C4 C3 C2 122.34(13) . . ?
C4 C3 C8 118.62(13) . . ?
C2 C3 C8 119.04(12) . . ?
C5 C4 C3 120.77(14) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 120.42(14) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 120.18(14) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C8 120.89(15) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C7 C8 C9 122.69(13) . . ?
C7 C8 C3 119.11(13) . . ?
C9 C8 C3 118.21(12) . . ?
C10 C9 C8 121.32(13) . . ?
C10 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
C9 C10 C1 121.78(13) . . ?
C9 C10 H10 119.1 . . ?
C1 C10 H10 119.1 . . ?
 
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
C10 C1 C2 C3 -0.8(2) . . . . ?
C1 C1 C2 C3 179.46(14) 3_666 . . . ?
C1 C2 C3 C4 -179.82(12) . . . . ?
C1 C2 C3 C8 0.9(2) . . . . ?
C2 C3 C4 C5 -179.48(13) . . . . ?
C8 C3 C4 C5 -0.2(2) . . . . ?
C3 C4 C5 C6 0.2(2) . . . . ?
C4 C5 C6 C7 -0.5(2) . . . . ?
C5 C6 C7 C8 0.8(2) . . . . ?
C6 C7 C8 C9 179.60(14) . . . . ?
C6 C7 C8 C3 -0.8(2) . . . . ?
C4 C3 C8 C7 0.5(2) . . . . ?
C2 C3 C8 C7 179.77(12) . . . . ?
C4 C3 C8 C9 -179.91(12) . . . . ?
C2 C3 C8 C9 -0.59(19) . . . . ?
C7 C8 C9 C10 179.92(13) . . . . ?
C3 C8 C9 C10 0.3(2) . . . . ?
C8 C9 C10 C1 -0.2(2) . . . . ?
C2 C1 C10 C9 0.5(2) . . . . ?
C1 C1 C10 C9 -179.78(14) 3_666 . . . ?
 
_refine_diff_density_max    0.241
_refine_diff_density_min   -0.173
_refine_diff_density_rms    0.037



