Redox-induced reversible [2 + 2] cycloaddition of an etheno-fused diporphyrin
Miyagawa, Kazuya; Hisaki, Ichiro; Fukui, Norihito; Shinokubo, Hiroshi; Chemical Science 12 (2021) 5224–5229; doi:10.1039/D1SC00438G

data_1560622
_publ_section_title
;
 Redox-induced reversible [2 + 2] cycloaddition of an etheno-fused
 diporphyrin
;
_journal_issue                   14
_journal_name_full               'Chemical Science'
_journal_page_first              5224
_journal_page_last               5229
_journal_paper_doi               10.1039/D1SC00438G
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C212 H200 N16 Ni4, 6(C7 H8)'
_chemical_formula_sum            'C254 H248 N16 Ni4'
_chemical_formula_weight         3759.51
_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-2018/3
_audit_update_record
;
2021-01-13 deposited with the CCDC.	2021-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                104.279(2)
_cell_angle_beta                 98.423(2)
_cell_angle_gamma                111.649(2)
_cell_formula_units_Z            2
_cell_length_a                   21.0654(6)
_cell_length_b                   22.4572(6)
_cell_length_c                   25.0542(7)
_cell_measurement_reflns_used    32157
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7990
_cell_measurement_theta_min      1.5890
_cell_volume                     10298.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Yadokari-XG 2009(Wakita Nemoto et al.)'
_computing_publication_material  'Yadokari-XG 2009(Wakita,Nemoto et al.)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_device_type  'SPring-8 BL40XU, Pilatus100K, DECTRIS'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.81104
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.1005
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            117152
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        29.119
_diffrn_reflns_theta_max         31.467
_diffrn_reflns_theta_min         1.594
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78403
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3992
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.654
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2453
_refine_ls_number_reflns         38537
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0926
_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^)+(0.1632P)^2^+3.4308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2561
_refine_ls_wR_factor_ref         0.2855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23793
_reflns_number_total             38537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00438g2.cif
_cod_data_source_block           KM200214_a
_cod_depositor_comments
'Adding full bibliography for 1560621--1560622.cif.'
_cod_original_cell_volume        10298.3(5)
_cod_database_code               1560622
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              4405
_shelx_hkl_checksum              10401