Easy and quantitative access to Fe(II) and Fe(III) di(aryl)alkynylphosphine oxides featuring [Fe(dppe)Cp*] endgroups: terminal P[double bond, length as m-dash]O functionality blocks the dimerisation of the Fe(III) derivatives
Ayham Tohme; Charles T. Hagen; Stephanie Essafi (nee Labouille); Arnaud Bondon; Thierry Roisnel; Duncan Carmichael; Frederic Paul; Chem.Commun. 51 (2015) 1316–; doi:10.1039/C4cc08993F

data_7116350
_publ_section_title
;
 Easy and quantitative access to Fe(II) and Fe(III)
 di(aryl)alkynylphosphine oxides featuring [Fe(dppe)Cp*] endgroups:
 terminal P[double bond, length as m-dash]O functionality blocks the
 dimerisation of the Fe(III) derivatives
;
_journal_name_full               Chem.Commun.
_journal_page_first              1316
_journal_paper_doi               10.1039/C4cc08993F
_journal_volume                  51
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C52 H53 Fe O P3'
_chemical_formula_sum            'C52 H53 Fe O P3'
_chemical_formula_weight         842.7
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_update_record
;
2014-07-23 deposited with the CCDC.
2014-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                76.510(2)
_cell_angle_beta                 77.792(2)
_cell_angle_gamma                69.833(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9336(4)
_cell_length_b                   13.3435(5)
_cell_length_c                   16.5675(6)
_cell_measurement_reflns_used    5773
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.57
_cell_measurement_theta_min      2.17
_cell_measurement_wavelength     0.71073
_cell_volume                     2183.44(14)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_av_unetI/netI     0.064
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30051
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         9891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.063
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.4900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                7561
_reflns_number_total             9891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc08993f2.cif
_cod_data_source_block           CTH25
_cod_database_code               7116350