Diversity-oriented synthesis of tetrathia[8]circulenes by sequential C-H borylation and annulation
Shohei Kato; Yuma Serizawa; Daisuke Sakamaki; Shu Seki; Yoshihiro Miyake; Hiroshi Shinokubo; Chem.Commun. 51 (2015) 16944–; doi:10.1039/C5cc06921A

data_7118097
_publ_section_title
;
 Diversity-oriented synthesis of tetrathia[8]circulenes by sequential C-H
 borylation and annulation
;
_journal_name_full               Chem.Commun.
_journal_page_first              16944
_journal_paper_doi               10.1039/C5cc06921A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C47 H67 B4 O8 S4'
_chemical_formula_weight         931.48
_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_update_record
;
2015-08-03 deposited with the CCDC.
2015-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                76.272(2)
_cell_angle_beta                 81.959(2)
_cell_angle_gamma                78.768(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2323(6)
_cell_length_b                   13.9489(7)
_cell_length_c                   16.2345(8)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    93.(2)
_cell_measurement_theta_max      28.6339
_cell_measurement_theta_min      2.5958
_cell_volume                     2626.6(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc.)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18066
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             994
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.162
_refine_diff_density_min         -0.491
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+5.1023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                7780
_reflns_number_total             8799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc06921a2.cif
_cod_data_source_block           I
_cod_database_code               7118097
_shelx_res_checksum              82441
_shelx_hkl_checksum              13901