Iridium Phosphite-Oxazoline Catalysts for the Highly Enantioselective Hydrogenation of Terminal Alkenes
Javier Mazuela; J. Johan Verendel; Mercedes Coll; Benjamín Schäffner; Armin Börner; Pher G. Andersson; Oscar Pàmies; Montserrat Diéguez; Journal of the American Chemical Society 131 (2009) 12344–12353; doi:10.1021/ja904152r

data_4104939
_publ_section_title
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 Iridium Phosphite-Oxazoline Catalysts for the Highly Enantioselective
 Hydrogenation of Terminal Alkenes
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12344
_journal_page_last               12353
_journal_paper_doi               10.1021/ja904152r
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration rm
_chemical_formula_sum            'C81 H80 B F24 Ir N O4 P'
_chemical_formula_weight         1821.44
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 97.396(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2560(12)
_cell_length_b                   41.907(5)
_cell_length_c                   18.538(2)
_cell_measurement_reflns_used    8921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.13
_cell_measurement_theta_min      2.60
_cell_volume                     7901.3(16)
_computing_cell_refinement       'Bruker APEX2 v2009.1-0'
_computing_data_collection       'Bruker APEX2 v2009.1-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -74
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            194514
_diffrn_reflns_theta_full        39.53
_diffrn_reflns_theta_max         39.53
_diffrn_reflns_theta_min         2.60
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           70
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    1.817
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7521
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         8.414
_refine_diff_density_min         -2.461
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.059(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2096
_refine_ls_number_reflns         73138
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0642P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                61684
_reflns_number_total             73138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja904152r_si_001.cif
_cod_data_source_block           op001_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_diffrn_measurement_specimen_suppport' was replaced with
'_diffrn_measurement_specimen_support' as specified in the
replacement file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_original_cell_volume        7901.5(16)
_cod_database_code               4104939