Dihydrogen Activation by a Diruthenium Analogue of the Fe-Only Hydrogenase Active Site
Aaron K. Justice; Rachel C. Linck; Thomas B. Rauchfuss; Scott R. Wilson; Journal of the American Chemical Society 126 (2004) 13214–13215; doi:10.1021/ja0455594

data_4113043
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Dihydrogen Activation by a Diruthenium Analogue of the Fe-Only
 Hydrogenase Active Site
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13214
_journal_page_last               13215
_journal_paper_doi               10.1021/ja0455594
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C42 H74 O3 P2 Ru2 S2, C6 H14'
_chemical_formula_sum            'C48 H88 O3 P2 Ru2 S2'
_chemical_formula_weight         1041.38
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_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
_audit_update_record
; 
2004-03-22   text and data added, rcl 
;
_cell_angle_alpha                75.717(4)
_cell_angle_beta                 86.966(5)
_cell_angle_gamma                89.780(4)
_cell_formula_units_Z            4
_cell_length_a                   15.304(4)
_cell_length_b                   18.602(4)
_cell_length_c                   19.048(4)
_cell_measurement_reflns_used    972
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.8
_cell_measurement_theta_min      2.5
_cell_volume                     5247(2)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.10 (Bruker, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL V6.10 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.10 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  p98zas
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2418
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30413
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0.3
_diffrn_standards_interval_time  306
_diffrn_standards_number         151
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.9574
_exptl_absorpt_correction_T_min  0.7828
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       tabular
_exptl_crystal_F_000             2200
_exptl_crystal_id                p98zas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0 -1 0) scattering planes 
roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.853
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1150
_refine_ls_number_reflns         30407
_refine_ls_number_restraints     418
_refine_ls_restrained_S_all      0.849
_refine_ls_R_factor_all          0.1727
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                13480
_reflns_number_total             30407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0455594si20040723_123438.cif
_cod_data_source_block           p98zas
_cod_original_cell_volume        5248(2)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4113043