Synthesis, Characterization, and Reactivity of Fe Complexes Containing Cyclic Diazadiphosphine Ligands: The Role of the Pendant Base in Heterolytic Cleavage of H2
Tianbiao Liu; Shentan Chen; Molly J. O'Hagan; Mary Rakowski DuBois; R. Morris Bullock; Daniel L. DuBois; Journal of the American Chemical Society 134 (2012) 6257–6272; doi:10.1021/ja211193j

data_4117769
_publ_contact_author
; 
Tianbiao Leo Liu 
Pacific Northwest National Laboratory 
Richland, WA, 99354 
USA 
;
_publ_contact_author_email       Tianbiao.Liu@pnl.gov
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of Fe Complexes Containing
 Cyclic Diazadiphosphine Ligands: The Role of the Pendant Base in
 Heterolytic Cleavage of H2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6257
_journal_page_last               6272
_journal_paper_doi               10.1021/ja211193j
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C67 H51 B F24 Fe N2 P2'
_chemical_formula_weight         1468.70
_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
_cell_angle_alpha                98.679(17)
_cell_angle_beta                 100.617(19)
_cell_angle_gamma                100.169(17)
_cell_formula_units_Z            2
_cell_length_a                   13.223(5)
_cell_length_b                   15.446(5)
_cell_length_c                   16.748(6)
_cell_measurement_reflns_used    8683
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.21
_cell_volume                     3249(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0718
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56416
_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.9580
_exptl_absorpt_correction_T_min  0.9470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         4.472
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.348
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         16204
_refine_ls_number_restraints     688
_refine_ls_restrained_S_all      2.318
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0959
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.5069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1839
_refine_ls_wR_factor_ref         0.1911
_reflns_number_gt                11106
_reflns_number_total             16204
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211193j_si_002_3.cif
_cod_data_source_block           1-H2
_cod_original_cell_volume        3249.5(19)
_cod_database_code               4117769