Weakly coordinating counter-ions for highly efficient catalysis of intramolecular hydroamination
Dabb, Serin L.; Ho, Joanne H. H.; Hodgson, Richard; Messerle, Barbara A.; Wagler, Jörg; Dalton Transactions  (2009) 634–; doi:10.1039/b814168a

data_7000374
_publ_section_title
;
 Weakly coordinating counter-ions for highly efficient catalysis of
 intramolecular hydroamination
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              634
_journal_paper_doi               10.1039/b814168a
_journal_year                    2009
_chemical_formula_moiety         'C32 H12 B F24, C17 H24 Ir N4'
_chemical_formula_sum            'C49 H36 B F24 Ir N4'
_chemical_formula_weight         1339.85
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.8340(10)
_cell_angle_beta                 64.3060(10)
_cell_angle_gamma                75.4040(10)
_cell_formula_units_Z            4
_cell_length_a                   17.0661(2)
_cell_length_b                   18.5517(2)
_cell_length_c                   19.3024(2)
_cell_measurement_reflns_used    130100
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.546
_cell_volume                     5003.69(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius Collect, KappaCCD'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP32 for windows (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa 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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            135754
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    2.798
_exptl_absorpt_correction_T_max  0.560
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.907
_refine_diff_density_min         -2.236
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.251
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1445
_refine_ls_number_reflns         29145
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.277
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+37.8737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1218
_reflns_number_gt                24977
_reflns_number_total             29145
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b814168a.txt
_cod_data_source_block           rh00701
_cod_original_cell_volume        5003.69(10)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000374