Amidine Dications: Isolation and [Fe]-Hydrogenase-Related Hydrogenation
Michael J. Corr; Kirsty F. Gibson; Alan R. Kennedy; John A. Murphy; Journal of the American Chemical Society 131 (2009) 9174–9175; doi:10.1021/ja9035847

data_4104656
_publ_section_title
;
 Amidine Dications: Isolation and [Fe]-Hydrogenase-Related Hydrogenation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9174
_journal_page_last               9175
_journal_paper_doi               10.1021/ja9035847
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C11 H15 F6 N3 O6 S2'
_chemical_formula_weight         463.38
_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                 95.355(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3365(8)
_cell_length_b                   14.1848(12)
_cell_length_c                   13.2684(10)
_cell_measurement_reflns_used    6668
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.67
_cell_measurement_theta_min      2.79
_cell_volume                     1749.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Xcalibur S'
_diffrn_measurement_method       '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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16299
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.72
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_description       'chunk cut from LARGE prism'
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0641P)^2^+0.4941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                4112
_reflns_number_total             4957
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja9035847_si_002_2.cif
_cod_data_source_block           jam0408
_cod_database_code               4104656