Synthesis, characterization and diastereoselective coordination of a planarly chiral, hybrid ferrocene ligand, (Sp)-2-(diphenylphosphino)ferrocenecarboxylic acid
Štěpnička, Petr; New Journal of Chemistry 26 (2002) 567–; doi:10.1039/b109495p

data_7050771
_publ_section_title
;
 Synthesis, characterization and diastereoselective coordination of a
 planarly chiral, hybrid ferrocene ligand,
 (Sp)-2-(diphenylphosphino)ferrocenecarboxylic acid
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              567
_journal_paper_doi               10.1039/b109495p
_journal_volume                  26
_journal_year                    2002
_chemical_formula_moiety         'C33H32ClFeO2PRu * 0.7 CH2Cl2'
_chemical_formula_sum            'C33.7 H33.4 Cl2.4 Fe O2 P Ru'
_chemical_formula_weight         743.37
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      92
_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.
_cell_angle_beta                 90.
_cell_angle_gamma                90.
_cell_formula_units_Z            8
_cell_length_a                   23.9653(2)
_cell_length_b                   23.9653(2)
_cell_length_c                   11.3015(1)
_cell_measurement_reflns_used    115407
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     6490.85(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 0.110
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method
;
CCD
(rotation scans, rotation per image 1.4\% \w,
exposure per frame 210 s, 350 images collected)
;
_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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            90352
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.188
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'rusty orange'
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3019
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         5727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0930P)^2^+6.5210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1460
_reflns_number_gt                5328
_reflns_number_total             5727
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109495p.txt
_cod_data_source_block           cyrupfc
_cod_original_cell_volume        6490.9(1)
_cod_original_sg_symbol_H-M      P41212
_cod_original_formula_sum        'C33.70 H33.40 Cl2.40 Fe O2 P Ru'
_cod_database_code               7050771