A Cyclodextrin Host/Guest Approach to a Hydrogenase Active Site Biomimetic Cavity
Michael L. Singleton; Joseph H. Reibenspies; Marcetta Y. Darensbourg; Journal of the American Chemical Society 132 (2010) 8870–8871; doi:10.1021/ja103774j

data_4102633
_publ_section_title
;
 A Cyclodextrin Host/Guest Approach to a Hydrogenase Active Site
 Biomimetic Cavity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8870
_journal_page_last               8871
_journal_paper_doi               10.1021/ja103774j
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C22 H24 Fe2 N2 O9 S3'
_chemical_formula_weight         668.31
_chemical_name_common            TEA1
_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                 99.752(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.1279(2)
_cell_length_b                   7.6853(5)
_cell_length_c                   16.7425(10)
_cell_measurement_reflns_used    2531
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      21.20
_cell_measurement_theta_min      2.47
_cell_volume                     2806.1(2)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4854
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    1.308
_exptl_absorpt_correction_T_max  0.9870
_exptl_absorpt_correction_T_min  0.8803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'red       '
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'needle    '
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.0010(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0503P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                4045
_reflns_number_total             4889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja103774j_si_004.cif
_cod_data_source_block           TEA1
_cod_database_code               4102633