Coordination Chemistry of the Soft Chiral Lewis Acid [Cp*Ir(TsDPEN)]+
Christopher S. Letko; Zachariah M. Heiden; Thomas B. Rauchfuss; Scott R. Wilson; Inorganic Chemistry 50 (2011) 5558–5566; doi:10.1021/ic200160q

data_4325390
_publ_contact_author
;
Christopher S. Letko 
University of Illinois 
School of Chemical Sciences, Box 80-6 
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 

Thomas B. Rauchfuss 
University of Illinois 
School of Chemical Sciences 
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
 

Scott R. Wilson 

University of Illinois 

School of Chemical Sciences, Box 59-1 

505 South Mathews Avenue 

Urbana, Illinois  61801 

USA 

;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Coordination Chemistry of the Soft Chiral Lewis Acid [Cp*Ir(TsDPEN)]+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5558
_journal_page_last               5566
_journal_paper_doi               10.1021/ic200160q
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '4(C32 H36 Ir n3 O2 S), 2(C H2 Cl2), H2 O'
_chemical_formula_sum            'C130 H150 Cl4 Ir4 O9 S4 n12'
_chemical_formula_weight         3063.46
_chemical_name_systematic
; 

? 

;
_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
_audit_update_record
; 

2008-03-10   text and data added, csl 

;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.1430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.6893(6)
_cell_length_b                   31.9208(12)
_cell_length_c                   15.4428(6)
_cell_measurement_reflns_used    4580
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      19.04
_cell_measurement_theta_min      2.35
_cell_volume                     6513.8(5)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 

SAINT V7.23A, XPREP V2005/2, SADABS V2007/4 (Bruker, 2005 & 2007) 

;
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2005)'
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ga73vas
_diffrn_reflns_av_R_equivalents  0.1201
_diffrn_reflns_av_sigmaI/netI    0.1180
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            59218
_diffrn_reflns_theta_full        25.61
_diffrn_reflns_theta_max         25.61
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    4.279
_exptl_absorpt_correction_T_max  0.9193
_exptl_absorpt_correction_T_min  0.5958
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       platy
_exptl_crystal_F_000             3052
_exptl_crystal_id                ga73vas
_exptl_crystal_preparation
; 

The data crystal was mounted using oil (Parantone-N, Exxon) to a 

0.3 mm cryo-loop (Hampton Research) with the (-1 6 -2) scattering 

planes roughly normal to the spindle axis. 

;
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.370
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         12221
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                6798
_reflns_number_total             12221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200160q_si_002_1.cif
_cod_data_source_block           ga73vas
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C130 H150 Cl4 Ir4 n12 O9 S4'
_cod_database_code               4325390