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_4133111
_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         'C98.38 H114.46 Cl12 N16.83 O6 Pd6'
_chemical_formula_sum            'C98.38 H114.46 Cl12 N16.83 O6 Pd6'
_chemical_formula_weight         2692.57
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.9770(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   19.5974(2)
_cell_length_b                   51.9761(6)
_cell_length_c                   14.24210(14)
_cell_measurement_reflns_used    65414
_cell_measurement_temperature    93
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      1.97
_cell_volume                     14504.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS Version 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       69
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            115408
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.633
_diffrn_reflns_theta_min         2.534
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5402.20
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.76
_refine_diff_density_min         -3.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1238
_refine_ls_number_reflns         35475
_refine_ls_number_restraints     299
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0948
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0454P)^2^+179.6339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2199
_refine_ls_wR_factor_ref         0.2259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30042
_reflns_number_total             35475
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja8b08534_si_004.cif
_cod_data_source_block           1@MMF
_cod_database_code               4133111
_shelx_res_checksum              24349
_shelx_hkl_checksum              3377
_shelx_fab_checksum              69386