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_4072398
_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            'C51 H66 Fe O P2 Pt'
_chemical_formula_weight         1007.92
_chemical_name_common            'complex 4b'
_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            4
_cell_length_a                   10.46390(10)
_cell_length_b                   17.2101(2)
_cell_length_c                   25.5495(3)
_cell_measurement_temperature    113(2)
_cell_volume                     4601.08(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            49777
_diffrn_reflns_theta_full        28.54
_diffrn_reflns_theta_max         28.54
_diffrn_reflns_theta_min         2.28
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.457
_exptl_absorpt_correction_T_max  0.8741
_exptl_absorpt_correction_T_min  0.4236
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.928
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         11538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                10485
_reflns_number_total             11538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8008316_si_002.cif
_cod_data_source_block           takada2
_cod_database_code               4072398