Tailored trisubstituted chiral Cp <sup> <i>x</i> </sup> Rh<sup>III</sup> catalysts for kinetic resolutions of phosphinic amides.
Sun, Y.; Cramer, N.; Chemical science 9 (2018) 2981–2985; doi:10.1039/c7sc05411d

data_1548872
_publ_section_title
;
 Tailored trisubstituted chiral Cp <sup> <i>x</i> </sup> Rh<sup>III</sup>
 catalysts for kinetic resolutions of phosphinic amides.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              2981
_journal_page_last               2985
_journal_paper_doi               10.1039/c7sc05411d
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H12 F6 N O P'
_chemical_formula_sum            'C15 H12 F6 N O P'
_chemical_formula_weight         367.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2017-11-29 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.7242(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.17707(14)
_cell_length_b                   8.43885(15)
_cell_length_c                   18.8541(3)
_cell_measurement_reflns_used    12173
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.5740
_cell_measurement_theta_min      4.4170
_cell_volume                     1585.46(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     17.00  42.00   1.00    3.77    --   50.00  79.00-104.24   25
  2  \w     28.00  60.00   1.00    3.77    --   58.00  74.00 -74.87   32
  3  \w     34.00  72.00   1.00    3.77    --   66.00  77.00 -71.31   38
  4  \w     95.00 132.00   1.00    3.77    --   58.00  74.00 -74.87   37
  5  \w     95.00 126.00   1.00    3.77    --   62.00  76.00-127.59   31
  6  \w    124.00 149.00   1.00    3.77    --   74.00  77.00-173.31   25
  7  \w    131.00 158.00   1.00   15.07    --  112.00  61.00-120.00   27
  8  \w    118.00 176.00   1.00   15.07    --  112.00  77.00-180.00   58
  9  \w    113.00 178.00   1.00   15.07    --  112.00  77.00-150.00   65
 10  \w    112.00 144.00   1.00   15.07    --   98.00  74.00 -18.80   32
 11  \w    113.00 140.00   1.00   15.07    --  112.00  77.00  60.00   27
 12  \w    115.00 178.00   1.00   15.07    --  112.00  77.00  90.00   63
 13  \w    103.00 131.00   1.00    3.77    --   66.00  77.00 135.24   28
 14  \w     95.00 144.00   1.00    3.77    --   70.00  77.00  65.22   49
 15  \w     89.00 138.00   1.00    3.77    --   66.00  76.00 176.98   49
 16  \w     84.00 110.00   1.00   15.07    --  112.00  61.00  90.00   26
 17  \w     83.00 113.00   1.00   15.07    --  112.00  61.00 120.00   30
 18  \w     80.00 158.00   1.00   15.07    --  112.00  77.00 150.00   78
 19  \w     85.00 120.00   1.00   15.07    --  112.00  61.00   0.00   35
 20  \w     84.00 113.00   1.00   15.07    --  112.00  61.00 -60.00   29
 21  \w     82.00 110.00   1.00   15.07    --  112.00  77.00-120.00   28
 22  \w     83.00 110.00   1.00   15.07    --  112.00  61.00-120.00   27
 23  \w     83.00 113.00   1.00   15.07    --  112.00  61.00-150.00   30
 24  \w     79.00 105.00   1.00   15.07    --  112.00  77.00 -90.00   26
 25  \w     83.00 177.00   1.00   15.07    --  112.00  61.00 -90.00   94
 26  \w     79.00 177.00   1.00   15.07    --  112.00  77.00  30.00   98
 27  \w     79.00 178.00   1.00   15.07    --  112.00  77.00 120.00   99
 28  \w     80.00 105.00   1.00   15.07    --  112.00  77.00  90.00   25
 29  \w     79.00 105.00   1.00   15.07    --  112.00  77.00  60.00   26
 30  \w     79.00 178.00   1.00   15.07    --  112.00  77.00   0.00   99
 31  \w     79.00 105.00   1.00   15.07    --  112.00  77.00-180.00   26
 32  \w     79.00 105.00   1.00   15.07    --  112.00  77.00-150.00   26
 33  \w     79.00 178.00   1.00   15.07    --  112.00  77.00 -60.00   99
 34  \w     66.00 111.00   1.00   15.07    --   98.00  74.00 -18.80   45
 35  \w     38.00  80.00   1.00    3.77    --   70.00  76.00  -2.95   42
 36  \w     37.00  77.00   1.00    3.77    --   70.00  77.00  65.22   40
 37  \w     32.00  63.00   1.00    3.77    --   62.00  76.00  23.26   31
 38  \w     31.00  56.00   1.00    3.77    --   62.00  75.00 -25.77   25
 39  \w     20.00  45.00   1.00    3.77    --   54.00  81.00 -25.90   25
 40  \w     -1.00  25.00   1.00    3.77    --   38.00  94.00 -17.87   26
 41  \w     30.00  57.00   1.00    3.77    --   62.00  76.00-127.59   27
 42  \w     38.00  70.00   1.00    3.77    --   70.00  77.00-125.80   32
 43  \w     41.00  74.00   1.00    3.77    --   74.00  77.00-173.31   33
 44  \w     20.00  45.00   1.00    3.77    --   54.00  81.00  58.76   25
 45  \w     28.00  55.00   1.00    3.77    --   58.00  76.00 108.61   27
 46  \w     33.00  62.00   1.00    3.77    --   66.00  77.00 135.24   29
 47  \w     34.00  60.00   1.00    3.77    --   66.00  76.00 176.98   26
 48  \w     11.00  37.00   1.00    3.77    --   46.00  84.00 176.10   26
 49  \w    -87.00 -13.00   1.00    3.77    --  -40.66 -57.00  60.00   74
 50  \w     24.00  92.00   1.00    3.77    --   40.66-125.00   0.00   68
 51  \w     38.00 108.00   1.00   15.07    --  112.00 -94.00  30.00   70
 52  \w     30.00 105.00   1.00   15.07    --  112.00 -94.00 120.00   75
 53  \w     23.00  80.00   1.00    3.77    --   40.66-125.00 150.00   57
 54  \w     31.00 109.00   1.00   15.07    --  112.00 -94.00 -60.00   78
 55  \w     96.00 121.00   1.00   15.07    --  112.00-125.00-180.00   25
 56  \w     59.00  86.00   1.00   15.07    --  112.00-125.00-180.00   27
 57  \w     31.00 105.00   1.00   15.07    --  112.00 -94.00-150.00   74
 58  \w    -69.00  32.00   1.00    3.77    --  -40.66  57.00-120.00  101
 59  \w   -109.00 -13.00   1.00    3.77    --  -40.66 -57.00 -90.00   96
 60  \w   -107.00 -17.00   1.00    3.77    --  -40.66 -57.00 150.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26120
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.240
_diffrn_reflns_theta_min         4.437
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.195
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.155
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 2519 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         6410
_refine_ls_number_restraints     575
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+0.8411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                6065
_reflns_number_total             6410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc05411d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 1548872--1548873.cif.'
_cod_original_cell_volume        1585.46(5)
_cod_database_code               1548872
_shelx_shelxl_version_number     2016/4
_shelx_res_checksum              85861