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_4334152
_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            'C66 H96 B Fe N2 P4'
_chemical_formula_weight         1107.99
_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                79.842(5)
_cell_angle_beta                 75.048(5)
_cell_angle_gamma                83.820(5)
_cell_formula_units_Z            2
_cell_length_a                   12.7369(11)
_cell_length_b                   14.0990(13)
_cell_length_c                   17.5151(17)
_cell_measurement_reflns_used    4451
_cell_measurement_temperature    154(2)
_cell_measurement_theta_max      20.518
_cell_measurement_theta_min      2.144
_cell_volume                     2984.8(5)
_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      154(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0880
_diffrn_reflns_av_sigmaI/netI    0.1280
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39524
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  0.9904
_exptl_absorpt_correction_T_min  0.9341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       'Thin plates'
_exptl_crystal_F_000             1194
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         10247
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.0696
_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^+0.1885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.2126
_reflns_number_gt                5668
_reflns_number_total             10247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3024953_si_001_4.cif
_cod_data_source_block           Complex3[BPh4]
_cod_database_code               4334152