Direct Observation of the Labile Imine Formation through Single-Crystal-to-Single-Crystal Reactions in the Pores of a Porous Coordination Network
Tsuyoshi Haneda; Masaki Kawano; Takehide Kawamichi; Makoto Fujita; Journal of the American Chemical Society 130 (2008) 1578–1579; doi:10.1021/ja7111564

data_4107397
_publ_contact_author             'Masaki Kawano'
_publ_contact_author_email       mkawano@appchem.t.u-tokyo.ac.jp
_publ_section_title
;
 Direct Observation of the Labile Imine Formation through
 Single-Crystal-to-Single-Crystal Reactions in the Pores of a Porous
 Coordination Network
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1578
_journal_page_last               1579
_journal_paper_doi               10.1021/ja7111564
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C66 H48 I6 N13 O2.5 Zn3'
_chemical_formula_weight         2020.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.280(3)
_cell_length_b                   14.012(2)
_cell_length_c                   44.907(5)
_cell_measurement_reflns_used    8626
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      23.137
_cell_measurement_theta_min      2.317
_cell_volume                     17795(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker XSHELL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker SMART CCD area detector system'
_diffrn_measurement_method       omega_scan
_diffrn_radiation_monochromator  'focusing mirror'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            206011
_diffrn_reflns_theta_full        29.01
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    2.926
_exptl_absorpt_correction_T_max  0.8440
_exptl_absorpt_correction_T_min  0.7203
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       needle
_exptl_crystal_F_000             7704
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.930
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1140
_refine_ls_number_reflns         22619
_refine_ls_number_restraints     1703
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1259P)^2^+95.6781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2101
_refine_ls_wR_factor_ref         0.2398
_reflns_number_gt                14374
_reflns_number_total             22619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7111564-file004_4.cif
_cod_data_source_block           1_p_anis
_cod_original_formula_sum        'C66 H48 I6 N13 O2.50 Zn3'
_cod_database_code               4107397