Proton-induced lewis acidity of unsaturated iridium amides.
Heiden, Zachariah M; Rauchfuss, Thomas B; Journal of the American Chemical Society 128 (2006) 13048–13049; doi:10.1021/ja0653831

data_4101383
_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_section_title
;
 Proton-induced lewis acidity of unsaturated iridium amides.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13048
_journal_page_last               13049
_journal_paper_doi               10.1021/ja0653831
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety
; 
C32 H12 B F24, C31 H36 Ir N2 O2 S, 2.5(C4 H10 O), H2 O 
;
_chemical_formula_sum            'C73 H75 B F24 Ir N2 O5.5 S'
_chemical_formula_weight         1759.42
_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
; 
2006-08-17   text and data added, zmh 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.430(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.585(5)
_cell_length_b                   25.611(6)
_cell_length_c                   15.358(4)
_cell_measurement_reflns_used    1021
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      20.49
_cell_measurement_theta_min      2.51
_cell_volume                     8258(3)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_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 0.996
_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  g76lasxt
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0650
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            64869
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.743
_exptl_absorpt_correction_T_max  0.6871
_exptl_absorpt_correction_T_min  0.5063
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3540
_exptl_crystal_id                g76lasxt
_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 0 1) scattering planes 
roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.982
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1487
_refine_ls_number_reflns         15140
_refine_ls_number_restraints     3898
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+18.1582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                10123
_reflns_number_total             15140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0653831si20060824_042659.cif
_cod_data_source_block           g76lasxt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c  '
_cod_original_formula_sum        'C73 H75 B F24 Ir N2 O5.50 S'
_cod_database_code               4101383