Electron-Rich Piano-Stool Iron σ-Acetylides Bearing a Functional Aryl Group. Synthesis and Characterization of Iron(II) and Iron(III) Complexes†
Denis, Raphaël; Toupet, Loïc; Paul, Frédéric; Lapinte, Claude; Organometallics 19 (2000) 4240–; doi:10.1021/om000325o

data_4077518
_publ_contact_author
;
Toupet Loic
G.M.C.M.-UMR6626
Universite de Rennes
Campus de Beaulieu
35042 RENNES cedex , FRANCE
;
_publ_section_title
;
 Electron-Rich Piano-Stool Iron \s-Acetylides Bearing a Functional Aryl
 Group. Synthesis and Characterization of Iron(II) and Iron(III)
 Complexes&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4240
_journal_paper_doi               10.1021/om000325o
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C44 H43 Fe N O2 P2'
_chemical_formula_weight         735.58
_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                95.110(2)
_cell_angle_beta                 105.910(2)
_cell_angle_gamma                116.590(3)
_cell_formula_units_Z            2
_cell_length_a                   12.131(3)
_cell_length_b                   12.190(3)
_cell_length_c                   15.223(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1876.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6872
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.525
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0122(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.7368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                4999
_reflns_number_total             6533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000325o.cif
_cod_data_source_block           compound_3a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077518