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_4325394
_publ_contact_author
; 

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         'C62 H72 Ir2 Mo n4 O4 S6, 2(C3 H6 O)'
_chemical_formula_sum            'C68 H84 Ir2 Mo O6 S6 n4'
_chemical_formula_weight         1726.09
_chemical_name_systematic
; 

? 

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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
; 

2008-09-02   text and data added, zmh 

;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.079(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.892(7)
_cell_length_b                   17.396(5)
_cell_length_c                   34.306(9)
_cell_measurement_reflns_used    5989
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      19.97
_cell_measurement_theta_min      2.24
_cell_volume                     14818(7)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  g49vast
_diffrn_reflns_av_R_equivalents  0.1114
_diffrn_reflns_av_sigmaI/netI    0.1139
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            72349
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        11.7
_diffrn_standards_interval_time  407
_diffrn_standards_number         213
_exptl_absorpt_coefficient_mu    3.968
_exptl_absorpt_correction_T_max  0.9234
_exptl_absorpt_correction_T_min  0.3699
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       platy
_exptl_crystal_F_000             6880
_exptl_crystal_id                g49vast
_exptl_crystal_preparation
; 

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

0.3 mm cryo-loop (Hampton Research) with the (0 0 -1) scattering 

planes roughly normal to the spindle axis. 

;
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.937
_refine_diff_density_min         -1.710
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     960
_refine_ls_number_reflns         13549
_refine_ls_number_restraints     1078
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                7756
_reflns_number_total             13549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200160q_si_002_5.cif
_cod_data_source_block           g49vast
_cod_original_cell_volume        14817(7)
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C68 H84 Ir2 Mo n4 O6 S6'
_cod_database_code               4325394