Catalytic hydrogen production by a Ni-Ru mimic of NiFe hydrogenases involves a proton-coupled electron transfer step
Sigolene Canaguier; Vincent Fourmond; Carlo U. Perotto; Jennifer Fize; Jacques Pecaut; Marc Fontecave; Martin J. Field; Vincent Artero; Chem.Commun. 49 (2013) 5004–; doi:10.1039/c3cc40987b

data_7109326
_publ_section_title
;
 Catalytic hydrogen production by a Ni-Ru mimic of NiFe hydrogenases
 involves a proton-coupled electron transfer step
;
_journal_name_full               Chem.Commun.
_journal_page_first              5004
_journal_paper_doi               10.1039/c3cc40987b
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C29 H44 Cl3 N Ni O3 Ru S4'
_chemical_formula_weight         849.02
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.2379(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   46.2747(7)
_cell_length_b                   17.1931(2)
_cell_length_c                   18.3604(4)
_cell_measurement_reflns_used    20649
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3363
_cell_measurement_theta_min      3.4033
_cell_volume                     13951.5(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
1 omega -46.00 50.00 0.7500 6.0000
omega____ theta____ kappa____ phi______ frames
- 25.4051 -37.0000 -90.0000 128
2 omega -5.00 94.00 0.7500 6.0000
omega____ theta____ kappa____ phi______ frames
- 25.4051 77.0000 150.0000 132
3 omega -10.00 76.25 0.7500 6.0000
omega____ theta____ kappa____ phi______ frames
- 25.4051 -116.0000 -100.0000 115
4 omega 0.00 95.25 0.7500 6.0000
omega____ theta____ kappa____ phi______ frames
- 25.4051 37.0000 90.0000 127
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54853
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_T_max  0.8465
_exptl_absorpt_correction_T_min  0.4235
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long plate'
_exptl_crystal_F_000             6976
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.491
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         17280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                12131
_reflns_number_total             17280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40987b.txt
_cod_data_source_block           sc140909
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7109326