Lewis Base Adducts Derived from Transfer Hydrogenation Catalysts: Scope and Selectivity
Heiden, Zachariah M.; Gorecki, Bradford J.; Rauchfuss, Thomas B.; Organometallics 27 (2008) 1542–; doi:10.1021/om700996m

data_4070762
_publ_contact_author
; 
Bradford J. Gorecki 
University of Illinois 
School of Chemical Sciences, Box 79-6 
600 South Mathews Ave 
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_section_title
;
 Lewis Base Adducts Derived from Transfer Hydrogenation Catalysts: Scope
 and Selectivity
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1542
_journal_paper_doi               10.1021/om700996m
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C24 H34 Ir N2 O3 S, B F4'
_chemical_formula_sum            'C24 H34 B F4 Ir N2 O3 S'
_chemical_formula_weight         709.60
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           1
_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
_audit_update_record
; 
2006-08-21 text and data added, bjg 
;
_cell_angle_alpha                91.517(3)
_cell_angle_beta                 99.724(3)
_cell_angle_gamma                97.879(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7323(5)
_cell_length_b                   10.0866(5)
_cell_length_c                   14.1647(7)
_cell_measurement_reflns_used    7142
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      29.88
_cell_measurement_theta_min      2.45
_cell_volume                     1355.82(12)
_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      297(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  ga75las
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33451
_diffrn_reflns_theta_full        30.61
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    5.057
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3171
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             700
_exptl_crystal_id                ga75las
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (2 -2 -7) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.249
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack (1983),  6665 Friedels'
_refine_ls_abs_structure_Flack   0.039(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         15092
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                13323
_reflns_number_total             15092
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700996m-file003.cif
_cod_data_source_block           ga75las
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     'P 1 '
_cod_original_sg_symbol_H-M      'P 1  '
_cod_database_code               4070762