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_1555862
_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            'C104 H96 N8 O4'
_chemical_formula_weight         1521.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 119.019(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   50.360(7)
_cell_length_b                   16.491(2)
_cell_length_c                   26.798(4)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.470
_cell_measurement_theta_min      2.318
_cell_volume                     19461(5)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.968
_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  0.0544
_diffrn_reflns_av_unetI/netI     0.0838
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            51868
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.525
_diffrn_reflns_theta_min         1.319
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;    
 SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_description       block
_exptl_crystal_F_000             6464
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.000324(14)
_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   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1066
_refine_ls_number_reflns         21689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0815
_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^)+(0.0100P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11674
_reflns_number_total             21689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b02761_si_004.cif
_cod_data_source_block           uch4mer_sqd
_cod_original_cell_volume        19462(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1555862
_shelxl_version_number           2014-3
_shelx_res_checksum              15566
_shelx_hkl_checksum              83820