Iridium Models of Rhodium Intermediates in Hydroformylation Catalysis: Isolation and Molecular Structures of Fluxional ae and ee Isomers
Abkai, Golnar; Schmidt, Sebastian; Rosendahl, Tobias; Rominger, Frank; Hofmann, Peter; Organometallics 33 (2014) 3212–; doi:10.1021/om401139u

data_4083551
_publ_section_title
;
 Iridium Models of Rhodium Intermediates in Hydroformylation Catalysis:
 Isolation and Molecular Structures of Fluxional ae and ee Isomers
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3212
_journal_paper_doi               10.1021/om401139u
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C68 H61 Ir O8 P2'
_chemical_formula_weight         1260.31
_chemical_name_common            'ae resting state'
_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
_cell_angle_alpha                67.531(1)
_cell_angle_beta                 76.095(1)
_cell_angle_gamma                77.868(1)
_cell_formula_units_Z            2
_cell_length_a                   11.4608(8)
_cell_length_b                   15.0988(11)
_cell_length_c                   18.7293(14)
_cell_measurement_reflns_used    9394
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.39
_cell_measurement_theta_min      2.20
_cell_volume                     2881.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II Quazar'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'ImuS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36113
_diffrn_reflns_theta_full        26.76
_diffrn_reflns_theta_max         26.76
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    2.429
_exptl_absorpt_correction_T_max  0.9307
_exptl_absorpt_correction_T_min  0.8110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen,             Germany.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.213
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         12273
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0351P)^2^+0.3703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0844
_reflns_number_gt                9959
_reflns_number_total             12273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401139u_si_002.cif
_cod_data_source_block           ga23
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4083551.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083551