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_4107395
_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            'C64.2 H47 I6 N13 O0.7 Zn3'
_chemical_formula_weight         1969.26
_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                   28.40(1)
_cell_length_b                   13.872(6)
_cell_length_c                   44.18(2)
_cell_measurement_reflns_used    9108
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      25.129
_cell_measurement_theta_min      2.333
_cell_volume                     17405(13)
_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 0.948
_diffrn_measured_fraction_theta_max 0.948
_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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            147657
_diffrn_reflns_theta_full        29.02
_diffrn_reflns_theta_max         29.02
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    2.988
_exptl_absorpt_correction_T_max  0.8411
_exptl_absorpt_correction_T_min  0.7157
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       needle
_exptl_crystal_F_000             7494
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.745
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         21965
_refine_ls_number_restraints     970
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+68.4565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.1896
_reflns_number_gt                15325
_reflns_number_total             21965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7111564-file004_2.cif
_cod_data_source_block           1_hex
_cod_original_formula_sum        'C64.20 H47 I6 N13 O0.70 Zn3'
_cod_database_code               4107395