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_4133109
_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         'C89.75 H96.62 Cl12 N14.87 O2 Pd6'
_chemical_formula_sum            'C89.75 H96.62 Cl12 N14.87 O2 Pd6'
_chemical_formula_weight         2479.41
_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                 90.911(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5614(5)
_cell_length_b                   51.550(2)
_cell_length_c                   14.2922(4)
_cell_measurement_reflns_used    19282
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.95
_cell_measurement_theta_min      2.09
_cell_volume                     14410.3(8)
_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 0.995
_diffrn_measured_fraction_theta_max 0.990
_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  0.0779
_diffrn_reflns_av_unetI/netI     0.1126
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       66
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            92855
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.536
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4941
_exptl_crystal_size_max          0.457
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.067
_refine_diff_density_max         3.188
_refine_diff_density_min         -2.291
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1074
_refine_ls_number_reflns         32808
_refine_ls_number_restraints     684
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.2288
_refine_ls_R_factor_gt           0.1763
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+708.0605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3660
_refine_ls_wR_factor_ref         0.3914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20058
_reflns_number_total             32808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08534_si_008.cif
_cod_data_source_block           afterIrradiation
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4133109
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.660
_shelx_estimated_absorpt_t_max   0.937
_shelx_res_checksum              58463
_shelx_hkl_checksum              87752
_shelx_fab_checksum              15102