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_1555861
_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            'C85 H80 N6 O3'
_chemical_formula_weight         1233.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.651(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.962(2)
_cell_length_b                   19.0061(18)
_cell_length_c                   15.2293(13)
_cell_measurement_reflns_used    6660
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.404
_cell_measurement_theta_min      2.174
_cell_volume                     6990.3(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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
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_diffrn_reflns_av_R_equivalents  0.1143
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            52890
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
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_diffrn_reflns_theta_max         23.257
_diffrn_reflns_theta_min         0.843
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;    
 SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       plate
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.0595
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6031
_reflns_number_total             10034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b02761_si_003.cif
_cod_data_source_block           209a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1555861
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              71959
_shelx_hkl_checksum              23084