Catalytic Arene H/D Exchange with Novel Rhodium and Iridium Complexes
Rhinehart, Jennifer L.; Manbeck, Kimberly A.; Buzak, Sara K.; Lippa, Geoffrey M.; Brennessel, William W.; Goldberg, Karen I.; Jones, William D.; Organometallics 31 (2012) 1943–; doi:10.1021/om2012419

data_4076483
_publ_section_title
;
 Catalytic Arene H/D Exchange with Novel Rhodium and Iridium Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1943
_journal_paper_doi               10.1021/om2012419
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C12 H15 Cl3 Ir N4 Na O2'
_chemical_formula_sum            'C12 H15 Cl3 Ir N4 Na O2'
_chemical_formula_weight         568.82
_chemical_name_common            Na-2
_chemical_name_systematic
; 
 [Ir(bdmpza)Cl3]Na 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5743(10)
_cell_length_b                   14.2503(17)
_cell_length_c                   13.7914(16)
_cell_measurement_reflns_used    4020
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      32.35
_cell_measurement_theta_min      3.14
_cell_volume                     1685.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0809
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39500
_diffrn_reflns_theta_full        37.78
_diffrn_reflns_theta_max         37.78
_diffrn_reflns_theta_min         2.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.436
_exptl_absorpt_correction_T_max  0.7190
_exptl_absorpt_correction_T_min  0.3020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.622
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         4649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0528P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                3236
_reflns_number_total             4649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2012419_si_002.cif
_cod_data_source_block           jonjlm19_Na-2
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4076483