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_1550166
_publ_section_title
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 Mild complexation protocol for chiral CpxRh and Ir complexes suitable for
 in situ catalysis
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04385J
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C22 H31 Ir O2'
_chemical_formula_sum            'C22 H31 Ir O2'
_chemical_formula_weight         519.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 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
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2018-09-26 deposited with the CCDC.
2018-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.0838(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8334(2)
_cell_length_b                   8.23239(14)
_cell_length_c                   22.2298(4)
_cell_measurement_reflns_used    14782
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.6880
_cell_measurement_theta_min      3.1170
_cell_volume                     1962.86(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    'Mercury 3.10 (Sheldrick, 2017)'
_computing_publication_material  'CIFTab (Sheldrick, 2015)'
_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 0.957
_diffrn_measurement_details
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List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -4.00  73.00   1.00    5.00    --   19.91  57.00 -30.00   77
  2  \w     -8.00  91.00   1.00    5.00    --   19.91  57.00-150.00   99
  3  \w     -9.00  96.00   1.00    5.00    --   19.91  77.00  60.00  105
  4  \w    -54.00  42.00   1.00    5.00    --   19.91 -38.00  60.00   96
  5  \w    -53.00  47.00   1.00    5.00    --   19.91 -57.00 -60.00  100
  6  \w    -49.00 -24.00   1.00    5.00    --   19.91 -38.00  30.00   25
  7  \w    -54.00  44.00   1.00    5.00    --   19.91 -38.00 150.00   98
  8  \w    -73.00 -39.00   1.00    5.00    --  -20.22 119.00  24.16   34
  9  \w    -97.00 -40.00   1.00    5.00    --  -20.22 155.00 140.87   57
;
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20184
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.878
_diffrn_reflns_theta_min         2.642
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.814
_exptl_absorpt_correction_T_max  0.474
_exptl_absorpt_correction_T_min  0.055
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.597
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 2805 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         6792
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0201P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0497
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.892
_reflns_number_gt                6580
_reflns_number_total             6792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04385j2.cif
_cod_data_source_block           bau-01-197
_cod_database_code               1550166
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.106
_shelx_estimated_absorpt_t_max   0.451
_shelx_res_checksum              77279
_publcif_funding_html
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