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_4325392
_publ_contact_author
;
Zachariah M. Heiden
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         'C30 H34 Ir n3 O4 S, C H2 Cl2'
_chemical_formula_sum            'C31 H36 Cl2 Ir O4 S n3'
_chemical_formula_weight         809.79
_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
; 

2007-04-19   text and data added, zmh 

;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.1970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1752(3)
_cell_length_b                   12.5127(2)
_cell_length_c                   17.3602(3)
_cell_measurement_reflns_used    7473
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.45
_cell_volume                     3165.56(10)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'APEX2 V1.0-27 (Bruker, 2004)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2001)'
_computing_publication_material  'XCIF (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  ga58ras
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48248
_diffrn_reflns_theta_full        27.69
_diffrn_reflns_theta_max         27.69
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    4.493
_exptl_absorpt_correction_T_max  0.7349
_exptl_absorpt_correction_T_min  0.3595
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       prism
_exptl_crystal_F_000             1608
_exptl_crystal_id                ga58ras
_exptl_crystal_preparation
; 

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

0.3 mm cryo-loop (Hampton Research) with the (9 -4 -6) scattering 

planes roughly normal to the spindle axis. 

;
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7264
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+2.0530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0513
_reflns_number_gt                5906
_reflns_number_total             7264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200160q_si_002_3.cif
_cod_data_source_block           ga58ras
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C31 H36 Cl2 Ir n3 O4 S'
_cod_database_code               4325392