m-Phenylene-Linked Dipyrrins and Their Boron-Difluoride Complexes as Variously Shaped Macrocyclic Oligomers.
Uchida, Junji; Nakamura, Takashi; Yamamura, Masaki; Yamaguchi, Gento; Nabeshima, Tatsuya; Organic letters 18 (2016) 5380–5383; doi:10.1021/acs.orglett.6b02761

data_1555860
_publ_section_title
;
 m-Phenylene-Linked Dipyrrins and Their Boron-Difluoride Complexes as
 Variously Shaped Macrocyclic Oligomers.
;
_journal_issue                   20
_journal_name_full               'Organic letters'
_journal_page_first              5380
_journal_page_last               5383
_journal_paper_doi               10.1021/acs.orglett.6b02761
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C116 H122 B2 F4 N8 O6'
_chemical_formula_weight         1821.83
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.715(6)
_cell_length_b                   32.715(6)
_cell_length_c                   20.819(4)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.07
_cell_measurement_theta_min      2.20
_cell_volume                     22282(7)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.583
_diffrn_measured_fraction_theta_max 0.999
_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  0.0505
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.583
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            88379
_diffrn_reflns_point_group_measured_fraction_full 0.576
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.779
_diffrn_reflns_theta_min         1.159
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6715
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       prism
_exptl_crystal_F_000             7744
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 4485 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_coef       0.00013(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1262
_refine_ls_number_reflns         11609
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0608P)^2^+12.0831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    0.567
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                10543
_reflns_number_total             11609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b02761_si_007.cif
_cod_data_source_block           c3_0m_sqd
_cod_original_cell_volume        22282(9)
_cod_database_code               1555860
_shelx_estimated_absorpt_t_min   0.989
_shelx_estimated_absorpt_t_max   0.996
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              3617
_shelx_hkl_checksum              33660