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_4076481
_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 H17 Cl3 Li N4 O3 Rh, C4 H8 O'
_chemical_formula_sum            'C16 H25 Cl3 Li N4 O4 Rh'
_chemical_formula_weight         553.60
_chemical_name_common            'Li-1 '
_chemical_name_systematic
; 
 [Rh(bdmpza)Cl3]Li.H2O
;
_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                 99.447(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3096(9)
_cell_length_b                   12.7502(14)
_cell_length_c                   20.107(2)
_cell_measurement_reflns_used    7044
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      37.46
_cell_measurement_theta_min      2.60
_cell_volume                     2101.4(4)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.1005
_diffrn_reflns_av_sigmaI/netI    0.0893
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            48567
_diffrn_reflns_theta_full        37.03
_diffrn_reflns_theta_max         37.03
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  0.9301
_exptl_absorpt_correction_T_min  0.7744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.378
_refine_diff_density_min         -1.478
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         10605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0300P)^2^+1.8228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                7044
_reflns_number_total             10605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2012419_si_002.cif
_cod_data_source_block           jonjlm12_Li-1
_cod_original_cell_volume        2101.5(4)
_cod_database_code               4076481