Synthesis and Coordination Behavior of Planar-Chiral Ferrocene Alkenylphosphines
Štěpnička, Petr; Císařová, Ivana; Inorganic Chemistry 45 (2006) 8785–8798; doi:10.1021/ic061278g

data_4333017
_publ_section_title
;
 Synthesis and Coordination Behavior of Planar-Chiral Ferrocene
 Alkenylphosphines
;
_journal_issue                   21
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8785
_journal_page_last               8798
_journal_paper_doi               10.1021/ic061278g
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C29 H23 Fe O4 P W'
_chemical_formula_sum            'C29 H23 Fe O4 P W'
_chemical_formula_weight         706.14
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                   10.7034(4)
_cell_length_b                   10.7034(4)
_cell_length_c                   46.411(2)
_cell_measurement_reflns_used    13951
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      2.58
_cell_volume                     5317.0(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.6876
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Oxford KM4 CCD diffractometer'
_diffrn_measurement_method       '\w and \p scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            29441
_diffrn_reflns_theta_full        26.59
_diffrn_reflns_theta_max         26.59
_diffrn_reflns_theta_min         2.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.962
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.
Version 1.171.29.8 (release 22-02-2006 CrysAlis171 .NET)
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)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.1418
_exptl_crystal_size_mid          0.0701
_exptl_crystal_size_min          0.0351
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5509
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0492
_reflns_number_gt                3987
_reflns_number_total             5509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061278gsup1.cif
_cod_data_source_block           ps167
_cod_original_sg_symbol_H-M      P41212
_cod_database_code               4333017