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_4117767
_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            'C35 H37 Cl Fe N2 P2'
_chemical_formula_weight         638.90
_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                109.293(2)
_cell_angle_beta                 102.347(2)
_cell_angle_gamma                93.685(2)
_cell_formula_units_Z            4
_cell_length_a                   10.8034(17)
_cell_length_b                   15.318(3)
_cell_length_c                   20.369(3)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.38
_cell_volume                     3074.5(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28331
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.7843
_exptl_absorpt_correction_T_min  0.7270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         12609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+1.0509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                10018
_reflns_number_total             12609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211193j_si_002_1.cif
_cod_data_source_block           1-Cl
_cod_original_cell_volume        3074.4(8)
_cod_database_code               4117767