The Complete Characterization of a Rhodium Lewis Acid-Dipolarophile Complex as an Intermediate for the Enantioselective Catalytic 1,3-Dipolar Cycloaddition of C,N-Diphenylnitrone to Methacrolein
Daniel Carmona; M. Pilar Lamata; Fernando Viguri; Ricardo Rodríguez; Luis A. Oro; Ana I. Balana; Fernando J. Lahoz; Tomás Tejero; Pedro Merino; Santiago Franco; Isabel Montesa; Journal of the American Chemical Society 126 (2004) 2716–2717; doi:10.1021/ja031995z

data_4112278
_publ_contact_author_address
;
  Dr. Fernando J. Lahoz
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       lahoz@posta.unizar.es
_publ_contact_author_fax         '+34 976 761187'
_publ_contact_author_name        'Dr. Fernando J. Lahoz'
_publ_contact_author_phone       '+34 976 761147'
_publ_section_title
;
 The Complete Characterization of a Rhodium Lewis Acid-Dipolarophile
 Complex as an Intermediate for the Enantioselective Catalytic 1,3-Dipolar
 Cycloaddition of C,N-Diphenylnitrone to Methacrolein
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2716
_journal_page_last               2717
_journal_paper_doi               10.1021/ja031995z
_journal_volume                  126
_journal_year                    2004
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C41 H47 O P2 Rh, 2(F6 Sb), C Cl2 H2'
_chemical_formula_sum            'C42 H49 Cl2 F12 O P2 Rh Sb2'
_chemical_formula_weight         1277.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.6002(14)
_cell_length_b                   13.6002(14)
_cell_length_c                   51.477(10)
_cell_measurement_reflns_used    28475
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.2605
_cell_volume                     9521(2)
_computing_cell_refinement       'SAINT+ v. 6.22 (Bruker AXS, 2001)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2001)'
_computing_data_reduction        'SAINT+ v. 6.22 (Bruker AXS, 2001)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.10 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.10 (Bruker, 2000)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            118669
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.55
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    1.728
_exptl_absorpt_correction_T_max  0.8129
_exptl_absorpt_correction_T_min  0.6768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; SADABS: Area-Detector Absorption Correction. Bruker-AXS 
  within SAINT+ package, v. 6.22 (2001).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             5024
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.125
_refine_diff_density_max         1.344
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.335
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         11785
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.335
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.122
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+29.3407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1159
_reflns_number_gt                11535
_reflns_number_total             11785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja031995zsi20040204_022051.cif
_cod_data_source_block           compound7
_cod_database_code               4112278