Rhodium-Catalyzed Enantioselective Hydrogenation of Unsaturated Phosphonates by Click Ferrophos Ligands
Takashi Konno; Kenta Shimizu; Kenichi Ogata; Shin-ichi Fukuzawa; Journal of Organic Chemistry 77 (2012) 3318–3324; doi:10.1021/jo300129m

data_4027114
_publ_section_title
;
 Rhodium-Catalyzed Enantioselective Hydrogenation of Unsaturated
 Phosphonates by Click Ferrophos Ligands
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3318
_journal_page_last               3324
_journal_paper_doi               10.1021/jo300129m
_journal_volume                  77
_journal_year                    2012
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C38 H33 Fe N3 P2'
_chemical_formula_sum            'C38 H33 Fe N3 P2'
_chemical_formula_weight         649.49
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_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.0888(17)
_cell_length_b                   16.229(3)
_cell_length_c                   19.287(4)
_cell_measurement_reflns_used    8941
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.17
_cell_volume                     3157.9(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24682
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.350
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3174 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.026(16)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         7205
_refine_ls_number_restraints     0
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_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0579P)^2^+3.9450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                6508
_reflns_number_total             7205
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo300129m_si_002.cif
_cod_data_source_block           20110727_konno_wcf2
_cod_original_cell_volume        3157.8(10)
_cod_database_code               4027114