Synthesis of Highly Twisted and Fully π-Conjugated Porphyrinic Oligomers.
Ito, Satoru; Hiroto, Satoru; Lee, Sangsu; Son, Minjung; Hisaki, Ichiro; Yoshida, Takuya; Kim, Dongho; Kobayashi, Nagao; Shinokubo, Hiroshi; Journal of the American Chemical Society 137 (2015) 142–145; doi:10.1021/ja511905f

data_4123221
_publ_section_title
;
 Synthesis of Highly Twisted and Fully \p-Conjugated Porphyrinic
 Oligomers.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              142
_journal_page_last               145
_journal_paper_doi               10.1021/ja511905f
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C60.57 H50 Cl18.28 N5 Ni'
_chemical_formula_weight         1554.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.121(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.296(4)
_cell_length_b                   22.701(5)
_cell_length_c                   35.704(7)
_cell_measurement_reflns_used    16185
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.4198
_cell_measurement_theta_min      3.0249
_cell_volume                     13911(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 63051
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            57974
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.9318
_exptl_absorpt_correction_T_min  0.8534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6297
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.250
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         12209
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1591P)^2^+61.0021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2311
_refine_ls_wR_factor_ref         0.2521
_reflns_number_gt                10675
_reflns_number_total             12209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja511905f_si_004.cif
_cod_data_source_block           121211
_cod_depositor_comments
'Adding full bibliography for 4123219--4123222.cif.'
_cod_original_cell_volume        13910(5)
_cod_database_code               4123221