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_4034093
_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         'C22 H25 Cl N Rh'
_chemical_formula_sum            'C22 H25 Cl N Rh'
_chemical_formula_weight         441.79
_chemical_name_common            Cp*RhCl(4-MePhPy)
_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             2018-09-05
_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                 93.030(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2807(7)
_cell_length_b                   7.7634(4)
_cell_length_c                   16.2421(8)
_cell_measurement_reflns_used    16423
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      33.0720
_cell_measurement_theta_min      2.7060
_cell_volume                     1924.11(16)
_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      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.874
_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    -32.00   3.00   0.50    1.62    --   10.95 -94.00  39.00   70
  2  \w    -26.00  20.00   0.50    1.62    --  -12.04 -99.00   0.00   92
  3  \w     10.00  41.00   0.50    1.62    --   10.95 -99.00 -60.00   62
  4  \w     40.00  70.00   0.50    1.62    --   10.95-178.00 -30.00   60
  5  \w    -25.00   7.00   0.50    1.62    --   10.95 -99.00 -60.00   64
  6  \w    -25.00  20.00   0.50    1.62    --  -12.04 -99.00-120.00   90
  7  \w    -33.00  -8.00   0.50    1.62    --  -12.04 -94.00  39.00   50
  8  \w     47.00  83.00   0.50    1.62    --   10.95-178.00 150.00   72
  9  \w    -62.00  32.00   0.50    1.62    --   10.95 -77.00-150.00  188
 10  \w    -38.00 -13.00   0.50    1.62    --  -12.04  94.00 150.00   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      0.0446449000
_diffrn_orient_matrix_UB_12      -0.0251252000
_diffrn_orient_matrix_UB_13      0.0034659000
_diffrn_orient_matrix_UB_21      0.0058123000
_diffrn_orient_matrix_UB_22      0.0307445000
_diffrn_orient_matrix_UB_23      -0.0404926000
_diffrn_orient_matrix_UB_31      0.0114878000
_diffrn_orient_matrix_UB_32      0.0822837000
_diffrn_orient_matrix_UB_33      0.0161933000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26225
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        29.575
_diffrn_reflns_theta_max         33.138
_diffrn_reflns_theta_min         2.511
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88256
_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    1.525
_exptl_crystal_description       needle
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         6419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0271P)^2^+0.9683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5739
_reflns_number_total             6419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b01716_si_002.cif
_cod_data_source_block           2g
_cod_database_code               4034093
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         RhClC22H25N
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.816
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.51
_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:
 C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;