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_4070765
_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_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         'C31 H39 Ir1 N3 O2 S, C2 H3 N, B F4'
_chemical_formula_sum            'C33 H42 B F4 Ir N4 O2 S'
_chemical_formula_weight         837.78
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_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
; 
2006-09-15   text and data added, zmh 
;
_cell_angle_alpha                94.397(2)
_cell_angle_beta                 97.846(2)
_cell_angle_gamma                105.071(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7300(4)
_cell_length_b                   10.8762(4)
_cell_length_c                   15.7950(6)
_cell_measurement_reflns_used    6011
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      28.81
_cell_measurement_theta_min      2.56
_cell_volume                     1751.08(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  ga51l_2as
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32096
_diffrn_reflns_theta_full        30.23
_diffrn_reflns_theta_max         30.23
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    3.928
_exptl_absorpt_correction_T_max  0.7923
_exptl_absorpt_correction_T_min  0.5970
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             836
_exptl_crystal_id                ga51l_2as
_exptl_crystal_preparation
; 
The data crystal was mounted using epoxy to a 0.3 mm cryo-loop 
(Hampton Research) with the (-1 -6 1) scattering planes roughly 
normal to the spindle axis. 
;
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.382
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         10373
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+0.9324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                8737
_reflns_number_total             10373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700996m-file003.cif
_cod_data_source_block           ga51l_2as
_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_cell_volume        1751.07(11)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1  '
_cod_database_code               4070765