Protonation of Ferrous Dinitrogen Complexes Containing a Diphosphine Ligand with a Pendent Amine
Zachariah M. Heiden; Shentan Chen; Michael T. Mock; William G. Dougherty; W. Scott Kassel; Roger Rousseau; R. Morris Bullock; Inorganic Chemistry 52 (2013) 4026–4039; doi:10.1021/ic4000704

data_4334372
_publ_section_title
;
 Protonation of Ferrous Dinitrogen Complexes Containing a Diphosphine
 Ligand with a Pendent Amine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4026
_journal_page_last               4039
_journal_paper_doi               10.1021/ic4000704
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C22 H54 Fe N2 P4'
_chemical_formula_weight         526.40
_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                88.390(4)
_cell_angle_beta                 89.899(4)
_cell_angle_gamma                85.777(4)
_cell_formula_units_Z            4
_cell_length_a                   10.2019(12)
_cell_length_b                   16.764(2)
_cell_length_c                   16.9450(19)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      32.98
_cell_measurement_theta_min      2.27
_cell_volume                     2889.0(6)
_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      110(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            60504
_diffrn_reflns_theta_full        33.24
_diffrn_reflns_theta_max         33.24
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.9283
_exptl_absorpt_correction_T_min  0.9016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       blade
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         21921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.3408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                15760
_reflns_number_total             21921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4000704_si_002_7.cif
_cod_data_source_block           pnl150
_cod_original_cell_volume        2888.9(6)
_cod_database_code               4334372