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_4084134
_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_formula_moiety         'C32 H40 N2 O2 Ru2, 2(F6 Sb), C H2 Cl2'
_chemical_formula_sum            'C33 H42 Cl2 F12 N2 O2 Ru2 Sb2'
_chemical_formula_weight         1243.23
_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                104.1610(10)
_cell_angle_beta                 93.3410(10)
_cell_angle_gamma                106.0270(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2673(8)
_cell_length_b                   12.6581(9)
_cell_length_c                   15.5594(11)
_cell_measurement_reflns_used    2373
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.212
_cell_measurement_theta_min      2.182
_cell_volume                     2049.1(3)
_computing_cell_refinement       'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, 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 0.997
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_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  0.1427
_diffrn_reflns_av_sigmaI/netI    0.1931
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19742
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.245
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.422
_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            orange
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.438
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.761
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         9186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.761
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1624
_reflns_number_gt                6112
_reflns_number_total             9186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5005463_si_002.cif
_cod_data_source_block           cmpnd_8c
_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 4084133--4084136.cif.
;
_cod_database_code               4084134