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_1550165
_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         'C25 H39 Ir O2 Si'
_chemical_formula_sum            'C25 H39 Ir O2 Si'
_chemical_formula_weight         591.85
_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   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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.70304(11)
_cell_length_b                   11.49824(16)
_cell_length_c                   26.9058(4)
_cell_measurement_reflns_used    30914
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.5960
_cell_measurement_theta_min      2.8770
_cell_volume                     2383.08(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.971
_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     26.00  93.00   1.00    3.00    --   19.91  57.00  60.00   67
  2  \w     39.00  90.00   1.00    3.00    --   19.91  38.00-120.00   51
  3  \w     -8.00  85.00   1.00    3.00    --   19.91  57.00-180.00   93
  4  \w    -13.00  95.00   1.00    3.00    --   19.91  77.00 -30.00  108
  5  \w    -20.00  61.00   1.00    3.00    --   19.91 -99.00-150.00   81
  6  \w    -46.00  44.00   1.00    3.00    --   19.91 -38.00  60.00   90
  7  \w    -53.00  53.00   1.00    3.00    --  -20.22  77.00 -90.00  106
  8  \w    -96.00 -57.00   1.00    3.00    --  -20.22 154.00  -7.16   39
  9  \w     38.00 107.00   1.00    3.00    --   19.91-178.00  90.00   69
;
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            51991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.981
_diffrn_reflns_theta_min         2.750
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.671
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.145
_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    1.650
_exptl_crystal_description       needle
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.829
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.151
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 3372 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(3)
_refine_ls_extinction_coef       0.00045(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         8448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0129P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0374
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                8176
_reflns_number_total             8448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04385j2.cif
_cod_data_source_block           shelx
_cod_database_code               1550165
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              56669