Intramolecular benzoallene–alkyne cycloaddition initiated by site-selective SN2’ reaction of epoxytetracene en route to π-extended pyracylene
Hamura, Toshiyuki; Kitamura, Kei; Asahina, Kenta; Adachi, Kazuhiko; Chemical Communications  (2019) –; doi:10.1039/C9CC05500B

data_7124059
_publ_section_title
;
 Intramolecular benzoallene--alkyne cycloaddition initiated by
 site-selective SN2&#x2019; reaction of epoxytetracene en route to
 \p-extended pyracylene
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05500B
_journal_year                    2019
_chemical_formula_sum            'C50 H27 Cl'
_chemical_formula_weight         663.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-10-02 deposited with the CCDC.    2019-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                92.409(6)
_cell_angle_beta                 91.727(7)
_cell_angle_gamma                104.223(7)
_cell_formula_units_Z            4
_cell_length_a                   10.264(5)
_cell_length_b                   14.861(8)
_cell_length_c                   24.721(11)
_cell_measurement_reflns_used    9563
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.7
_cell_volume                     3649(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            42434
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         1.415
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         16719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1542P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2024
_refine_ls_wR_factor_ref         0.2493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11364
_reflns_number_total             16719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05500b2.cif
_cod_data_source_block           aa_sqd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7124059
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.927
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              20609
_platon_squeeze_void_probe_radius 1.20