Mechanistic Insights of a Concerted Metalation‒Deprotonation Reaction with [Cp*RhCl2]2
Walsh, Aaron P.; Jones, William D.; Organometallics 34 (2015) 3400–; doi:10.1021/acs.organomet.5b00369

data_4086176
_publ_section_title
;
 Mechanistic Insights of a Concerted Metalation--Deprotonation Reaction
 with [Cp*RhCl2]2
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3400
_journal_paper_doi               10.1021/acs.organomet.5b00369
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C22 H25 Cl N O Rh'
_chemical_formula_sum            'C22 H25 Cl N O Rh'
_chemical_formula_weight         457.79
_chemical_name_common            jonaw65
_chemical_name_systematic
; 
 Cp*RhCl(4-MeOC6H3-Py)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 91.4942(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3174(13)
_cell_length_b                   16.2657(14)
_cell_length_c                   8.1709(7)
_cell_measurement_reflns_used    3954
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      38.46
_cell_measurement_theta_min      3.54
_cell_volume                     1902.2(3)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_laue_measured_fraction_full 0.988
_diffrn_reflns_laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23624
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        37.785
_diffrn_reflns_theta_max         38.582
_diffrn_reflns_theta_min         1.895
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.6377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
; 
 Flack x determined using 4545 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.011(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         10040
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0226
_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^)+(0.0216P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0504
_reflns_Friedel_coverage         0.936
_reflns_friedel_fraction_full    0.944
_reflns_friedel_fraction_max     0.904
_reflns_number_gt                9735
_reflns_number_total             10040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00369_si_002.cif
_cod_data_source_block           4
_cod_database_code               4086176
_shelx_estimated_absorpt_t_min   0.679
_shelx_estimated_absorpt_t_max   0.867
_shelxl_version_number           2013-4
_shelx_res_checksum              37859
_shelx_hkl_checksum              58524