Low Oxidation State Iron(0), Iron(I), and Ruthenium(0) Dinitrogen Complexes with a Very Bulky Neutral Phosphine Ligand
Ryan Gilbert-Wilson; Leslie D. Field; Stephen B. Colbran; Mohan M. Bhadbhade; Inorganic Chemistry 52 (2013) 3043–3053; doi:10.1021/ic3024953

data_4334153
_publ_section_title
;
 Low Oxidation State Iron(0), Iron(I), and Ruthenium(0) Dinitrogen
 Complexes with a Very Bulky Neutral Phosphine Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3043
_journal_page_last               3053
_journal_paper_doi               10.1021/ic3024953
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C44.5 H83 Cl P4 Ru'
_chemical_formula_weight         878.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 114.028(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.905(2)
_cell_length_b                   26.160(5)
_cell_length_c                   14.691(3)
_cell_measurement_reflns_used    1563
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      17.9115
_cell_measurement_theta_min      2.798
_cell_volume                     4880.9(16)
_computing_cell_refinement       '<i>APEX2 </i>(Bruker, 2007)'
_computing_data_collection       '<i>APEX2 </i>(Bruker, 2007)'
_computing_data_reduction        '<i>APEX2 </i>(Bruker, 2007)'
_computing_molecular_graphics    '<i>SHELXTL-Plus</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL-97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.1575
_diffrn_reflns_av_sigmaI/netI    0.1858
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35186
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.9857
_exptl_absorpt_correction_T_min  0.9048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            'Dark Blue'
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       'Triangular Prism'
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8604
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1778
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.4069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.2152
_reflns_number_gt                4191
_reflns_number_total             8604
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3024953_si_001_5.cif
_cod_data_source_block           Complex4
_cod_original_cell_volume        4880.9(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C44.50 H83 Cl P4 Ru'
_cod_database_code               4334153