Mechanistic Study of Acetate-Assisted C‒H Activation of 2-Substituted Pyridines with [MCl2Cp*]2(M = Rh, Ir) and [RuCl2(p-cymene)]2
Boutadla, Youcef; Al-Duaij, Omar; Davies, David L.; Griffith, Gerald A.; Singh, Kuldip; Organometallics 28 (2009) 433–440; doi:10.1021/om800909w

data_4063509
_publ_section_title
;
 Mechanistic Study of Acetate-Assisted C--H Activation of 2-Substituted
 Pyridines with [MCl2Cp*]2(M = Rh, Ir) and [RuCl2(p-cymene)]2
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              433
_journal_page_last               440
_journal_paper_doi               10.1021/om800909w
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C21 H23 Cl N Rh'
_chemical_formula_weight         427.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.644(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4528(13)
_cell_length_b                   14.780(3)
_cell_length_c                   16.956(3)
_cell_measurement_reflns_used    871
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.241
_cell_measurement_theta_min      2.462
_cell_volume                     1822.4(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14041
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 7479 reflections(SADABS);Rint 0.0470 before
correction and 0.0375 after.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                2996
_reflns_number_total             3580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800909w_si_002.cif
_cod_data_source_block           07026
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        1822.5(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4063509