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_4102632
_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_absolute_configuration rm
_chemical_formula_sum            'C98 H204 Fe2 N Na O107 S3'
_chemical_formula_weight         3339.49
_chemical_name_common            1-CyD
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.517(3)
_cell_angle_beta                 98.507(3)
_cell_angle_gamma                103.154(3)
_cell_formula_units_Z            1
_cell_length_a                   15.346(4)
_cell_length_b                   15.422(4)
_cell_length_c                   17.595(4)
_cell_measurement_reflns_used    3968
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      19.20
_cell_measurement_theta_min      2.14
_cell_volume                     3582.7(16)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.1510
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33320
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.9634
_exptl_absorpt_correction_T_min  0.8958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'colorless '
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate     '
_exptl_crystal_F_000             1766
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1958
_refine_ls_number_reflns         24259
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0930P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1797
_refine_ls_wR_factor_ref         0.2086
_reflns_number_gt                15725
_reflns_number_total             24259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja103774j_si_003.cif
_cod_data_source_block           1CyD
_cod_original_cell_volume        3582.9(15)
_cod_database_code               4102632