Mild complexation protocol for chiral CpxRh and Ir complexes suitable for in situ catalysis
Cramer, Nicolai; Audic, Benoit; Wodrich, Matthew D.; Chemical Science  (2019) –; doi:10.1039/C8SC04385J

data_1550167
_publ_section_title
;
 Mild complexation protocol for chiral CpxRh and Ir complexes suitable for
 in situ catalysis
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04385J
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C17 H28 O2 Si'
_chemical_formula_sum            'C17 H28 O2 Si'
_chemical_formula_weight         292.48
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-09-26 deposited with the CCDC.
2018-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.53335(13)
_cell_length_b                   10.27117(14)
_cell_length_c                   22.6089(3)
_cell_measurement_reflns_used    22925
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.4640
_cell_measurement_theta_min      3.8850
_cell_volume                     1749.39(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(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 0.996
_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     14.00  63.00   1.00    2.00    --   40.91  57.00 -30.00   49
  2  \w     86.00 133.00   1.00    2.00    --   58.00  76.00 -93.66   47
  3  \w     92.00 133.00   1.00    2.00    --   58.00  76.00 -46.37   41
  4  \w    137.00 178.00   1.00    8.00    --  107.03  77.00   0.00   41
  5  \w    122.00 148.00   1.00    8.00    --  107.03  77.00-120.00   26
  6  \w    127.00 153.00   1.00    8.00    --  107.03  77.00-180.00   26
  7  \w     79.00 137.00   1.00    8.00    --  107.03  61.00-150.00   58
  8  \w     79.00 138.00   1.00    8.00    --  107.03  61.00 -90.00   59
  9  \w    115.00 173.00   1.00    8.00    --  107.03  77.00 -30.00   58
 10  \w    117.00 164.00   1.00    8.00    --  107.03  77.00 120.00   47
 11  \w     75.00 167.00   1.00    8.00    --  107.03  77.00 150.00   92
 12  \w     78.00 111.00   1.00    8.00    --  107.03  61.00 150.00   33
 13  \w     74.00 100.00   1.00    8.00    --  107.03  77.00 120.00   26
 14  \w     75.00 170.00   1.00    8.00    --  107.03  77.00  90.00   95
 15  \w     81.00 110.00   1.00    8.00    --  107.03  61.00   0.00   29
 16  \w     75.00 171.00   1.00    8.00    --  107.03  77.00 -60.00   96
 17  \w     75.00 169.00   1.00    8.00    --  107.03  77.00 -90.00   94
 18  \w     80.00 105.00   1.00    8.00    --  107.03  61.00-180.00   25
 19  \w     79.00 104.00   1.00    8.00    --  107.03  61.00-120.00   25
 20  \w     74.00 100.00   1.00    8.00    --  107.03  77.00-180.00   26
 21  \w     75.00 176.00   1.00    8.00    --  107.03  77.00-150.00  101
 22  \w     74.00  99.00   1.00    8.00    --  107.03  77.00 -30.00   25
 23  \w     74.00 133.00   1.00    8.00    --  107.03  77.00   0.00   59
 24  \w     74.00 100.00   1.00    8.00    --  107.03  77.00-120.00   26
 25  \w     38.00  67.00   1.00    2.00    --   70.00  76.00  16.82   29
 26  \w     35.00  62.00   1.00    2.00    --   66.00  76.00  84.38   27
 27  \w     35.00  79.00   1.00    2.00    --   66.00  76.00 114.38   44
 28  \w     66.00 138.00   1.00    2.00    --   62.00  76.00 154.72   72
 29  \w     74.00 173.00   1.00    8.00    --  107.03  77.00  60.00   99
 30  \w     74.00 160.00   1.00    8.00    --  107.03  77.00  30.00   86
 31  \w     46.00 139.00   1.00    8.00    --  107.03 -77.00-120.00   93
 32  \w     47.00 107.00   1.00    8.00    --  107.03 -94.00-180.00   60
 33  \w     33.00  61.00   1.00    2.00    --   40.91-125.00-120.00   28
 34  \w      2.00  78.00   1.00    2.00    --   40.91 -99.00 -60.00   76
 35  \w     44.00 112.00   1.00    8.00    --  107.03-125.00  90.00   68
 36  \w     27.00  87.00   1.00    8.00    --  107.03 -94.00 120.00   60
 37  \w     27.00  52.00   1.00    2.00    --   58.00  76.00 -46.37   25
 38  \w     33.00  66.00   1.00    2.00    --   66.00  77.00 -18.19   33
 39  \w     34.00  67.00   1.00    2.00    --   66.00  77.00  47.64   33
 40  \w     30.00  56.00   1.00    2.00    --   62.00  76.00 -25.97   26
 41  \w     21.00  46.00   1.00    2.00    --   54.00  79.00 -66.63   25
 42  \w     20.00  45.00   1.00    2.00    --   54.00  81.00-105.03   25
 43  \w     26.00  52.00   1.00    2.00    --   58.00  76.00 -93.66   26
 44  \w     20.00  45.00   1.00    2.00    --   54.00  81.00-154.32   25
 45  \w     28.00  71.00   1.00    2.00    --   58.00  77.00-173.35   43
 46  \w     -4.00  23.00   1.00    2.00    --   34.00  91.00 -32.61   27
 47  \w     11.00  36.00   1.00    2.00    --   46.00  84.00  57.73   25
 48  \w     12.00  38.00   1.00    2.00    --   46.00  81.00 122.61   26
 49  \w     30.00  56.00   1.00    2.00    --   62.00  76.00 154.72   26
 50  \w    -56.00 -20.00   1.00    2.00    --  -40.91 -38.00-120.00   36
 51  \w     -5.00  24.00   1.00    2.00    --   34.00  94.00-167.61   29
 52  \w    -89.00 -12.00   1.00    2.00    --  -40.91 125.00  30.00   77
 53  \w   -123.00  36.00   1.00    2.00    --  -40.91   0.00   0.00  159
 54  \w   -111.00 -60.00   1.00    2.00    --  -40.91 -38.00-120.00   51
;
_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  0.0236
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28192
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.574
_diffrn_reflns_theta_min         3.910
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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    1.111
_exptl_crystal_description       prism
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.545
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.156
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
 Flack x determined using 1463 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.3648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0569
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                3490
_reflns_number_total             3520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04385j2.cif
_cod_data_source_block           shelx_CCDC1
_cod_database_code               1550167
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              57303