Chiral Brønsted Acid Catalysts. Activation of Methyl 3,3,3-Trifluoropyruvate by Hydroxymethylpyridine-Containing Half-Sandwich Complexes
Carmona, Daniel; Lamata, Pilar; Sánchez, Antonio; Pardo, Pilar; Rodríguez, Ricardo; Ramírez, Paola; Lahoz, Fernando J.; García-Orduña, Pilar; Oro, Luis A.; Organometallics 33 (2014) 4016–; doi:10.1021/om5005463

data_4084135
_publ_section_title
;
 Chiral Br\/onsted Acid Catalysts. Activation of Methyl
 3,3,3-Trifluoropyruvate by Hydroxymethylpyridine-Containing Half-Sandwich
 Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4016
_journal_paper_doi               10.1021/om5005463
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C39 H41 Ir N2 O3 P, F6 Sb'
_chemical_formula_sum            'C39 H41 F6 Ir N2 O3 P Sb'
_chemical_formula_weight         1044.66
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.282(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.972(2)
_cell_length_b                   9.467(2)
_cell_length_c                   19.936(4)
_cell_measurement_reflns_used    1134
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.358
_cell_measurement_theta_min      2.207
_cell_volume                     1874.1(7)
_computing_cell_refinement       'SAINT+ v. 5.65 (Bruker AXS, 2003)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 5.65 (Bruker AXS, 2003)'
_computing_molecular_graphics    'XP program, SHELXTL v.6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTL v 6.12, BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1196
_diffrn_reflns_av_sigmaI/netI    0.2165
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17019
_diffrn_reflns_theta_full        27.40
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.381
_exptl_absorpt_correction_T_max  0.8179
_exptl_absorpt_correction_T_min  0.5745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction (1996) Bruker-AXS
 within SAINT+ package, v. 6.45.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.091
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.748
_refine_diff_density_min         -2.365
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8045
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1688
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1758
_reflns_number_gt                4275
_reflns_number_total             8045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5005463_si_002.cif
_cod_data_source_block           cmpnd_11b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 4084133--4084136.cif.
;
_cod_original_cell_volume        1873.9(7)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4084135