Direct crystallographic observation of a coordinatively unsaturated transition-metal complex in situ generated within a self-assembled cage.
Kawano, Masaki; Kobayashi, Yasuhiro; Ozeki, Tomoji; Fujita, Makoto; Journal of the American Chemical Society 128 (2006) 6558–6559; doi:10.1021/ja0609250

data_4101272
_publ_contact_author             'Masaki Kawano'
_publ_section_title
;
 Direct crystallographic observation of a coordinatively unsaturated
 transition-metal complex in situ generated within a self-assembled
 cage.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6558
_journal_page_last               6559
_journal_paper_doi               10.1021/ja0609250
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C157.48 H111.92 Mn3.18 N45.66 O106.58 Pd6'
_chemical_formula_weight         5162.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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            4
_cell_length_a                   29.055(3)
_cell_length_b                   29.055(3)
_cell_length_c                   30.767(7)
_cell_measurement_reflns_used    9560
_cell_measurement_temperature    78(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      2.2
_cell_volume                     25973(7)
_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      78(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker SMART CCD area detector system'
_diffrn_measurement_method       omega_scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            304957
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.8980
_exptl_absorpt_correction_T_min  0.8345
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10339
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.126
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1192
_refine_ls_number_reflns         32145
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1633
_refine_ls_R_factor_gt           0.1022
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1540P)^2^+95.7395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2581
_refine_ls_wR_factor_ref         0.3117
_reflns_number_gt                20464
_reflns_number_total             32145
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0609250si20060208_045957.cif
_cod_data_source_block           Cage_CpMn
_cod_original_sg_symbol_H-M      P4(1)2(1)2
_cod_database_code               4101272