Asymmetric hydrogenation of an α-unsaturated carboxylic acid catalyzed by intact chiral transition metal carbonyl clusters - diastereomeric control of enantioselectivity.
Abdel-Magied, Ahmed F; Theibich, Yusuf; Singh, Amrendra K.; Rahaman, Ahibur; Doverbratt, Isa; Raha, Arun K.; Haukka, Matti; Richmond, Michael G.; Nordlander, Ebbe; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4244–4256; doi:10.1039/c9dt04799a

data_7703617
_publ_section_title
;
 Asymmetric hydrogenation of an \a-unsaturated carboxylic acid catalyzed
 by intact chiral transition metal carbonyl clusters - diastereomeric
 control of enantioselectivity.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4244
_journal_page_last               4256
_journal_paper_doi               10.1039/c9dt04799a
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C49 H38 Fe O7 P2 Ru3 S), 1/2(C4 H14)'
_chemical_formula_sum            'C101 H83 Fe2 O14 P4 Ru6 S2'
_chemical_formula_weight         2426.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-02-12 deposited with the CCDC.	2020-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.11044(17)
_cell_length_b                   20.7626(4)
_cell_length_c                   21.0868(4)
_cell_measurement_reflns_used    8760
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.6680
_cell_measurement_theta_min      2.1730
_cell_volume                     5302.15(16)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'UCSF Chimera (Petterssen et al. 2004)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25373
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.589
_diffrn_reflns_theta_min         1.939
_diffrn_source                   micro-source
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82651
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       needle
_exptl_crystal_F_000             2418
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 3997 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         14236
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.851
_reflns_number_gt                11461
_reflns_number_total             14236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04799a2.cif
_cod_data_source_block           af342w8
_cod_depositor_comments
'Adding full bibliography for 7703615--7703621.cif.'
_cod_original_cell_volume        5302.14(16)
_cod_database_code               7703617
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.723
_shelx_estimated_absorpt_t_max   0.942
_shelx_res_checksum              91889