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_4076482
_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 N4 O2 Rh, C8 H20 N'
_chemical_formula_sum            'C20 H35 Cl3 N5 O2 Rh'
_chemical_formula_weight         586.79
_chemical_name_common            Et4N-1
_chemical_name_systematic
; 
 [Rh(bdmpza)Cl3]Et4N 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.660(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.402(8)
_cell_length_b                   12.261(10)
_cell_length_c                   19.677(15)
_cell_measurement_reflns_used    1243
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      21.55
_cell_measurement_theta_min      2.59
_cell_volume                     2466(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.3145
_diffrn_reflns_av_sigmaI/netI    0.2505
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18744
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_T_max  0.9693
_exptl_absorpt_correction_T_min  0.8507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.746
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4363
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.2489
_refine_ls_R_factor_gt           0.1326
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2673
_refine_ls_wR_factor_ref         0.3113
_reflns_number_gt                1994
_reflns_number_total             4363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2012419_si_002.cif
_cod_data_source_block           jonjlm15_Et4N-1
_cod_database_code               4076482