Preferential Photoreaction in a Porous Crystal, Metal-Macrocycle Framework: Pd<sup>II</sup>-Mediated Olefin Migration over [2+2] Cycloaddition.
Yonezawa, Hirotaka; Tashiro, Shohei; Shiraogawa, Takafumi; Ehara, Masahiro; Shimada, Rintaro; Ozawa, Takeaki; Shionoya, Mitsuhiko; Journal of the American Chemical Society 140 (2018) 16610–16614; doi:10.1021/jacs.8b08534

data_4133112
_publ_section_title
;
 Preferential Photoreaction in a Porous Crystal, Metal-Macrocycle
 Framework: Pd<sup>II</sup>-Mediated Olefin Migration over [2+2]
 Cycloaddition.
;
_journal_issue                   48
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16610
_journal_page_last               16614
_journal_paper_doi               10.1021/jacs.8b08534
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C93.05 H109.57 Cl12 N16.53 O6 Pd6'
_chemical_formula_sum            'C93.05 H109.57 Cl12 N16.53 O6 Pd6'
_chemical_formula_weight         2619.36
_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-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90.818(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6067(4)
_cell_length_b                   51.7809(13)
_cell_length_c                   14.2567(3)
_cell_measurement_reflns_used    34685
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      2.08
_cell_volume                     14472.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.2'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS Version 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       67
_diffrn_reflns_limit_k_min       -64
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            137187
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.536
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5246
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.063
_refine_diff_density_max         3.783
_refine_diff_density_min         -3.332
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1127
_refine_ls_number_reflns         33116
_refine_ls_number_restraints     486
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.1793
_refine_ls_R_factor_gt           0.1544
_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^)+(0.0001P)^2^+661.6981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3196
_refine_ls_wR_factor_ref         0.3302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25280
_reflns_number_total             33116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08534_si_007.cif
_cod_data_source_block           beforeIrradiation
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4133112
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.670
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              94701
_shelx_hkl_checksum              34862
_shelx_fab_checksum              7607