Straightforward Access to Stable, 16-Valence-Electron Phosphine-Stabilized Fe0 Olefin Complexes and Their Reactivity
Burcher, Benjamin; Sanders, Kevin J.; Benda, Ladislav; Pintacuda, Guido; Jeanneau, Erwann; Danopoulos, Andreas A.; Braunstein, Pierre; Olivier-Bourbigou, Hélène; Breuil, Pierre-Alain R.; Organometallics 36 (2017) 605–; doi:10.1021/acs.organomet.6b00803

data_4087160
_publ_section_title
;
 Straightforward Access to Stable, 16-Valence-Electron
 Phosphine-Stabilized Fe0 Olefin Complexes and Their Reactivity
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              605
_journal_paper_doi               10.1021/acs.organomet.6b00803
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C50 H46 Fe N2 P4, 2(C7 H8)'
_chemical_formula_sum            'C64 H62 Fe N2 P4'
_chemical_formula_weight         1038.95
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                70.958(2)
_cell_angle_beta                 81.770(2)
_cell_angle_gamma                89.191(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2192(3)
_cell_length_b                   14.5626(4)
_cell_length_c                   17.5759(3)
_cell_measurement_reflns_used    11414
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.9790
_cell_measurement_theta_min      3.5300
_cell_volume                     2684.85(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9897
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36535
_diffrn_reflns_theta_full        26.331
_diffrn_reflns_theta_max         29.327
_diffrn_reflns_theta_min         3.179
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.178
_refine_diff_density_max         1.59
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9872
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         12679
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.0008848
_refine_ls_shift/su_mean         0.0000457
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 3.65P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1103
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1103
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              19
_reflns_limit_k_min              -17
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                10048
_reflns_number_total             12704
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.44
_oxford_diffrn_Wilson_scale      0.54
_oxford_refine_ls_r_factor_ref   0.0638
_oxford_refine_ls_scale          2.514(12)
_oxford_reflns_number_all        12679
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            om6b00803_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C64 H62 Fe1 N2 P4'
_cod_database_code               4087160
_oxdiff_exptl_absorpt_empirical_full_min 0.463
_oxdiff_exptl_absorpt_empirical_full_max 1.559
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;