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_4087161
_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         'C54 H52 Fe1 P4'
_chemical_formula_sum            'C54 H52 Fe P4'
_chemical_formula_weight         880.75
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 106.233(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.275(3)
_cell_length_b                   10.8131(12)
_cell_length_c                   17.896(2)
_cell_measurement_reflns_used    6795
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.8840
_cell_measurement_theta_min      3.2290
_cell_volume                     4324.4(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.161
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52320
_diffrn_reflns_theta_full        25.702
_diffrn_reflns_theta_max         29.679
_diffrn_reflns_theta_min         2.965
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.105
_refine_diff_density_max         2.21
_refine_diff_density_min         -1.43
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9216
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         8665
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0918
_refine_ls_shift/su_max          0.0003123
_refine_ls_shift/su_mean         0.0000422
_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: 
 417. 619. 321. 82.3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2907
_refine_ls_wR_factor_gt          0.2506
_refine_ls_wR_factor_ref         0.2907
_reflns_limit_h_max              30
_reflns_limit_h_min              -31
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                5727
_reflns_number_total             10776
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.85
_oxford_diffrn_Wilson_scale      0.86
_oxford_refine_ls_r_factor_ref   0.1300
_oxford_refine_ls_scale          0.692(3)
_oxford_reflns_number_all        8665
_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 21/c 1 '
_cod_original_formula_sum        'C54 H52 Fe1 P4'
_cod_database_code               4087161
_oxdiff_exptl_absorpt_empirical_full_min 0.860
_oxdiff_exptl_absorpt_empirical_full_max 2.121
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;