The Hydrophilic Phosphatriazaadamantane Ligand in the Development of H2 Production Electrocatalysts: Iron Hydrogenase Model Complexes
Rosario Mejia-Rodriguez; Daesung Chong; Joseph H. Reibenspies; Manuel P. Soriaga; Marcetta Y. Darensbourg; Journal of the American Chemical Society 126 (2004) 12004–12014; doi:10.1021/ja039394v

data_4112954
_publ_section_title
;
 The Hydrophilic Phosphatriazaadamantane Ligand in the Development of H2
 Production Electrocatalysts: Iron Hydrogenase Model Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12004
_journal_page_last               12014
_journal_paper_doi               10.1021/ja039394v
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C14 H18 Fe2 N3 O5 P S2'
_chemical_formula_weight         515.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.424(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8502(16)
_cell_length_b                   12.4174(18)
_cell_length_c                   13.1985(18)
_cell_measurement_reflns_used    818
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      45.97
_cell_measurement_theta_min      5.17
_cell_volume                     1936.4(5)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Multi-wire area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1219
_diffrn_reflns_av_sigmaI/netI    0.1412
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10087
_diffrn_reflns_theta_full        59.08
_diffrn_reflns_theta_max         59.08
_diffrn_reflns_theta_min         4.90
_exptl_absorpt_coefficient_mu    15.107
_exptl_absorpt_correction_T_max  0.5188
_exptl_absorpt_correction_T_min  0.3134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                1473
_reflns_number_total             2574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja039394vsi20031103_023251.cif
_cod_data_source_block           ddrr01
_cod_database_code               4112954