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_4101271
_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            'C142.75 H171.5 Mn3.84 N45.5 O97.25 Pd6'
_chemical_formula_weight         4929.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 99.5401(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.3225(4)
_cell_length_b                   45.7184(6)
_cell_length_c                   46.6645(7)
_cell_measurement_reflns_used    431
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      2
_cell_volume                     51173(2)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  Si
_diffrn_radiation_source         KEK
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68900
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_sigmaI/netI    0.1104
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            70062
_diffrn_reflns_theta_full        17.20
_diffrn_reflns_theta_max         17.20
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.9603
_exptl_absorpt_correction_T_min  0.9228
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green-yellow
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             19972
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.330
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3807
_refine_ls_number_reflns         33410
_refine_ls_number_restraints     5524
_refine_ls_restrained_S_all      1.441
_refine_ls_R_factor_all          0.1502
_refine_ls_R_factor_gt           0.1125
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3204
_refine_ls_wR_factor_ref         0.3445
_reflns_number_gt                21519
_reflns_number_total             33410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0609250si20060208_045957.cif
_cod_data_source_block           100k_on
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C142.75 H171.50 Mn3.84 N45.50 O97.25 Pd6'
_cod_database_code               4101271