Synthesis, Characterization, Properties, and Asymmetric Catalytic Diels−Alder Reactions of Chiral-at-Metal Phosphinooxazoline-Rhodium(III) and −Iridium(III) Complexes§
Carmona, Daniel; Lahoz, Fernando J.; Elipe, Sergio; Oro, Luis A.; Lamata, M. Pilar; Viguri, Fernando; Sánchez, Fernando; Martínez, Sonia; Cativiela, Carlos; López-Ram de Víu, M. Pilar; Organometallics 21 (2002) 5100–; doi:10.1021/om020582o

data_4077103
_publ_section_title
;
 Synthesis, Characterization, Properties, and Asymmetric Catalytic
 Diels&#x2212;Alder Reactions of Chiral-at-Metal
 Phosphinooxazoline-Rhodium(III) and &#x2212;Iridium(III)
 Complexes&#x00A7;
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5100
_journal_paper_doi               10.1021/om020582o
_journal_volume                  21
_journal_year                    2002
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C32 H35 Cl Ir N O P 1+, F6 Sb 1-'
_chemical_formula_sum            'C32 H35 Cl F6 Ir N O P Sb'
_chemical_formula_weight         943.98
_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                 101.129(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6110(10)
_cell_length_b                   14.2880(10)
_cell_length_c                   11.0420(10)
_cell_measurement_reflns_used    96
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      15
_cell_volume                     1642.6(2)
_computing_cell_refinement       'XSCANS v. 2.1 (Siemens)'
_computing_data_collection       'XSCANS v. 2.1 (Siemens)'
_computing_data_reduction        'XSCANS v. 2.1 (Siemens)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10,Bruker2000'
_computing_publication_material  'XCIF program, SHELXTL v6.10,Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'four circle diffractometer,Siemens P4'
_diffrn_measurement_method       '\w/2\q scans'
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8207
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.060
_exptl_absorpt_correction_T_max  0.208
_exptl_absorpt_correction_T_min  0.131
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 Azimuthal psi-scans of 15 reflections at 10\% intervals.
 Data corrected with the program XPREP (SHELXTL v. 5 Bruker)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.506
_refine_diff_density_min         -1.655
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(6)
_refine_ls_extinction_coef       0.0037(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         7515
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0743P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                7235
_reflns_number_total             7515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020582o.cif
_cod_data_source_block           compound6a
_cod_original_sg_symbol_H-M      P1211
_cod_database_code               4077103