Synthesis and Ligand Properties of 1-Phosphaethenyl-2-phosphanylferrocenes
Takita, Ryo; Takada, Yuko; Jensen, Rader S.; Okazaki, Masaaki; Ozawa, Fumiyuki; Organometallics 27 (2008) 6279–; doi:10.1021/om8008316

data_4072397
_publ_section_title
;
 Synthesis and Ligand Properties of
 1-Phosphaethenyl-2-phosphanylferrocenes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6279
_journal_paper_doi               10.1021/om8008316
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C45 H50 Fe P2'
_chemical_formula_weight         708.64
_chemical_name_common            'complex 3b'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.550(3)
_cell_length_b                   15.300(3)
_cell_length_c                   34.447(7)
_cell_measurement_temperature    173(2)
_cell_volume                     7668(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_sigmaI/netI    0.0854
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            62571
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.49
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.9800
_exptl_absorpt_correction_T_min  0.7857
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.019(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         17494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          3.057
_refine_ls_shift/su_mean         0.271
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+1.9818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                13618
_reflns_number_total             17494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8008316_si_001.cif
_cod_data_source_block           takada1
_cod_original_cell_volume        7669(3)
_cod_database_code               4072397