Reversible Concerted Metalation-Deprotonation C-H Bond Activation by [Cp*RhCl<sub>2</sub>]<sub>2</sub>.
VanderWeide, Andrew I.; Brennessel, William W.; Jones, William D.; The Journal of organic chemistry 84 (2019) 12960–12965; doi:10.1021/acs.joc.9b01716

data_4034095
_publ_section_title
;
 Reversible Concerted Metalation-Deprotonation C-H Bond Activation by
 [Cp*RhCl<sub>2</sub>]<sub>2</sub>.
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12960
_journal_page_last               12965
_journal_paper_doi               10.1021/acs.joc.9b01716
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C25 H31 Cl N Rh'
_chemical_formula_sum            'C25 H31 Cl N Rh'
_chemical_formula_weight         483.87
_chemical_name_common            Cp*RhCl(4-tBuPhPy)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-11-02
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.3440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7685(2)
_cell_length_b                   7.45310(10)
_cell_length_c                   16.4415(2)
_cell_measurement_reflns_used    10394
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.6410
_cell_measurement_theta_min      4.7610
_cell_volume                     2262.52(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.979
_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    -65.00 -39.00   0.50    0.17    --  -49.62  97.00-127.00   52
  2  \w    -72.00 -47.00   0.50    0.67    --  -84.25  97.00-127.00   50
  3  \w    -70.00  20.00   0.50    0.17    --  -49.62  77.00  60.00  180
  4  \w    -46.00 -13.00   0.50    0.67    --  -84.25  15.00  90.00   66
  5  \w     -5.00  79.00   0.50    0.17    --   49.62 -97.00 124.00  168
  6  \w     76.00 109.00   0.50    0.67    --  105.75 -97.00 124.00   66
  7  \w     69.00 109.00   0.50    0.67    --  105.75 -94.00  30.00   80
  8  \w     54.00 109.00   0.50    0.67    --  105.75-105.00  35.98  110
  9  \w     58.00  85.00   0.50    0.67    --  105.75 -45.00 -30.00   54
 10  \w     38.00  63.00   0.50    0.67    --  105.75-125.00-120.00   50
 11  \w     76.00 116.00   0.50    0.67    --  105.75-125.00-120.00   80
 12  \w     76.00 120.00   0.50    0.67    --  105.75 -61.00-180.00   88
 13  \w     56.00  82.00   0.50    0.67    --  105.75 -94.00-180.00   52
 14  \w     38.00  63.00   0.50    0.67    --  105.75 -61.00-180.00   50
 15  \w     36.00  68.00   0.50    0.67    --  105.75 -30.00-120.00   64
 16  \w     40.00  68.00   0.50    0.67    --  105.75 -15.00-180.00   56
 17  \w     34.00  67.00   0.50    0.67    --  105.75 -30.00-180.00   66
 18  \w     36.00  71.00   0.50    0.67    --  105.75 -15.00 -90.00   70
 19  \w     36.00  70.00   0.50    0.67    --  105.75 -30.00 -60.00   68
 20  \w     33.00  60.00   0.50    0.67    --  105.75 -15.00 -60.00   54
 21  \w     35.00  65.00   0.50    0.67    --  105.75 -30.00 -90.00   60
 22  \w     35.00  89.00   0.50    0.67    --  105.75 -45.00  30.00  108
 23  \w     42.00  67.00   0.50    0.67    --  105.75 -97.00 124.00   50
 24  \w     43.00 109.00   0.50    0.67    --  105.75 -94.00  60.00  132
 25  \w     43.00  69.00   0.50    0.67    --  105.75 -30.00  90.00   52
 26  \w     36.00  67.00   0.50    0.67    --  105.75 -30.00 120.00   62
 27  \w     37.00  74.00   0.50    0.67    --  105.75 -45.00  90.00   74
 28  \w    110.00 142.00   0.50    0.67    --  105.75  97.00-127.00   64
 29  \w    -22.00  56.00   0.50    0.17    --   49.62 -38.00-180.00  156
 30  \w   -117.00 -92.00   0.50    0.17    --  -49.62-125.00-180.00   50
 31  \w   -143.00-118.00   0.50    0.67    --  -84.25 -97.00 124.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0782820000
_diffrn_orient_matrix_UB_12      0.0077250000
_diffrn_orient_matrix_UB_13      0.0162146000
_diffrn_orient_matrix_UB_21      0.0018923000
_diffrn_orient_matrix_UB_22      0.2064148000
_diffrn_orient_matrix_UB_23      -0.0039697000
_diffrn_orient_matrix_UB_31      -0.0288013000
_diffrn_orient_matrix_UB_32      -0.0074009000
_diffrn_orient_matrix_UB_33      -0.0937768000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19287
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.967
_diffrn_reflns_theta_min         2.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.245
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.660
_refine_diff_density_min         -1.103
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0745P)^2^+2.0126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4341
_reflns_number_total             4750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b01716_si_002.cif
_cod_data_source_block           2i
_cod_original_cell_volume        2262.51(5)
_cod_database_code               4034095
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.327
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C)
;