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_4087157
_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         'C35 H44 Fe O P2 Si2'
_chemical_formula_sum            'C35 H44 Fe O P2 Si2'
_chemical_formula_weight         654.67
_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                76.850(3)
_cell_angle_beta                 74.749(3)
_cell_angle_gamma                69.161(4)
_cell_formula_units_Z            2
_cell_length_a                   11.8587(5)
_cell_length_b                   11.8767(4)
_cell_length_c                   13.4547(5)
_cell_measurement_reflns_used    10761
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.3040
_cell_measurement_theta_min      3.4500
_cell_volume                     1689.70(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 0.999
_diffrn_measured_fraction_theta_max 0.883
_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  0.042
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29805
_diffrn_reflns_theta_full        26.556
_diffrn_reflns_theta_max         29.349
_diffrn_reflns_theta_min         3.026
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.637
_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            black
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.482
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9628
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         8183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.0011606
_refine_ls_shift/su_mean         0.0000354
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.112E+04 0.160E+04 894. 300. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0820
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0819
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                6931
_reflns_number_total             8201
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.40
_oxford_diffrn_Wilson_scale      0.06
_oxford_refine_ls_r_factor_ref   0.0484
_oxford_refine_ls_scale          5.46(5)
_oxford_reflns_number_all        8184
_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_database_code               4087157
_oxdiff_exptl_absorpt_empirical_full_min 0.399
_oxdiff_exptl_absorpt_empirical_full_max 1.726
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;