Synthesis of figure-of-eight helical bisBODIPY macrocycles and their chiroptical properties.
Saikawa, Makoto; Nakamura, Takashi; Uchida, Junji; Yamamura, Masaki; Nabeshima, Tatsuya; Chemical communications (Cambridge, England) 52 (2016) 10727–10730; doi:10.1039/c6cc05439k

data_7124902
_publ_section_title
;
 Synthesis of figure-of-eight helical bisBODIPY macrocycles and their
 chiroptical properties.
;
_journal_issue                   71
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10727
_journal_page_last               10730
_journal_paper_doi               10.1039/c6cc05439k
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C61.5 H46.5 B Cl4.5 N4 O6'
_chemical_formula_weight         1107.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-17 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                75.181(3)
_cell_angle_beta                 83.052(4)
_cell_angle_gamma                88.030(3)
_cell_formula_units_Z            4
_cell_length_a                   13.411(3)
_cell_length_b                   20.416(5)
_cell_length_c                   21.320(5)
_cell_measurement_reflns_used    5972
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      21.914
_cell_measurement_theta_min      2.291
_cell_volume                     5602(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_unetI/netI     0.1538
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38088
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        21.984
_diffrn_reflns_theta_max         21.984
_diffrn_reflns_theta_min         0.995
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.4794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;    
 SADABS-2014/4 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1236
_refine_ls_number_reflns         13569
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1712
_refine_ls_R_factor_gt           0.0912
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1398P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2259
_refine_ls_wR_factor_ref         0.2635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6880
_reflns_number_total             13569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05439k2.cif
_cod_data_source_block           cycbmono
_cod_original_formula_sum        'C61.50 H46.50 B Cl4.50 N4 O6'
_cod_database_code               7124902
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              77254
_shelx_hkl_checksum              77010