X-Shaped Cyclobutane-Linked Tetraporphyrins through a Thermal [2+2] Cycloaddition of Etheno-Fused Diporphyrins.
Nagai, Tomohiro; Takiguchi, Asahi; Ueda, Masayuki; Oda, Kazuma; Hiroto, Satoru; Shinokubo, Hiroshi; Journal of the American Chemical Society 140 (2018) 8392–8395; doi:10.1021/jacs.8b04673

data_4132530
_publ_section_title
;
 X-Shaped Cyclobutane-Linked Tetraporphyrins through a Thermal [2+2]
 Cycloaddition of Etheno-Fused Diporphyrins.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8392
_journal_page_last               8395
_journal_paper_doi               10.1021/jacs.8b04673
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C141 H157 Cl15 N10 O0 Zn2'
_chemical_formula_weight         2654.25
_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   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                69.546(4)
_cell_angle_beta                 85.836(3)
_cell_angle_gamma                67.732(4)
_cell_formula_units_Z            2
_cell_length_a                   18.8651(7)
_cell_length_b                   19.7892(8)
_cell_length_c                   20.6097(8)
_cell_measurement_reflns_used    10559
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.8020
_cell_measurement_theta_min      1.9910
_cell_volume                     6655.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_publication_material  'CrystalStructure 4.2'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.1374
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46463
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.629
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.829
_refine_diff_density_min         -1.443
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1614
_refine_ls_number_reflns         23178
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1748
_refine_ls_R_factor_gt           0.0938
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1378P)^2^+14.3714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2328
_refine_ls_wR_factor_ref         0.2856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12608
_reflns_number_total             23178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04673_si_003.cif
_cod_data_source_block           nagai_170117_Zn_condens_single_bond_a
_cod_database_code               4132530
_oxdiff_exptl_absorpt_empirical_full_min 0.476
_oxdiff_exptl_absorpt_empirical_full_max 2.232
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_shelxl_version_number           2014-3
_shelx_res_checksum              47502
_shelx_hkl_checksum              61830