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_1550168
_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         'C40 H43 Ir O2 Si'
_chemical_formula_sum            'C40 H43 Ir O2 Si'
_chemical_formula_weight         776.03
_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   geom
_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                 102.019(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1531(2)
_cell_length_b                   14.0965(3)
_cell_length_c                   23.1228(6)
_cell_measurement_reflns_used    29042
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.3840
_cell_measurement_theta_min      2.8060
_cell_volume                     3236.86(13)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.915
_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    -13.00  86.00   1.00    6.44    --   11.66  38.00 -30.00   99
  2  \w      2.00  86.00   1.00    6.44    --   11.66  38.00  90.00   84
  3  \w    -12.00  42.00   1.00    6.44    --   11.66  38.00  60.00   54
  4  \w    -44.00  40.00   1.00    6.44    --   11.66 -57.00 -90.00   84
  5  \w    -20.00  53.00   1.00    6.44    --   11.66 -99.00  30.00   73
  6  \w      7.00  71.00   1.00    6.44    --   11.66-132.00 124.00   64
  7  \w    -21.00  86.00   1.00    6.44    --   11.66  77.00-180.00  107
  8  \w     43.00  98.00   1.00    6.44    --   11.66 178.00 -90.00   55
  9  \w    -84.00 -59.00   1.00    6.44    --  -11.97 149.00 115.81   25
;
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            54468
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.700
_diffrn_reflns_theta_min         2.517
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.197
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.028
_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    1.592
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.883
_exptl_crystal_size_mid          0.593
_exptl_crystal_size_min          0.118
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.516
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details
;
 Flack x determined using 6162 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         16010
_refine_ls_number_restraints     493
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+1.4529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.824
_reflns_number_gt                15075
_reflns_number_total             16010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04385j2.cif
_cod_data_source_block           shelx_CCDC2
_cod_original_cell_volume        3236.86(14)
_cod_database_code               1550168
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              19069