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_4101273
_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            'C8 H5 Mn O3'
_chemical_formula_weight         204.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 115.7200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7492(3)
_cell_length_b                   6.9262(2)
_cell_length_c                   11.6456(3)
_cell_measurement_reflns_used    6430
_cell_measurement_temperature    78(2)
_cell_measurement_theta_max      37.6
_cell_measurement_theta_min      3.4
_cell_volume                     781.13(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      78(2)
_diffrn_measured_fraction_theta_full 0.765
_diffrn_measured_fraction_theta_max 0.765
_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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12521
_diffrn_reflns_theta_full        37.61
_diffrn_reflns_theta_max         37.61
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.645
_exptl_absorpt_correction_T_max  0.8270
_exptl_absorpt_correction_T_min  0.5967
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         3170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0364P)^2^+0.1173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                2532
_reflns_number_total             3170
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0609250si20060208_045957.cif
_cod_data_source_block           CpMn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4101273