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_4077102
_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         'C34 H39 Cl Ir N O P 1+, B F4 1-'
_chemical_formula_sum            'C34 H39 B Cl F4 Ir N O P'
_chemical_formula_weight         823.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   11.7815(7)
_cell_length_b                   16.1335(10)
_cell_length_c                   17.2609(13)
_cell_measurement_reflns_used    88
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      10
_cell_volume                     3280.9(4)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9636
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.251
_exptl_absorpt_correction_T_max  0.427
_exptl_absorpt_correction_T_min  0.188
_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    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.586
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         8689
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0369P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                7531
_reflns_number_total             8689
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020582o.cif
_cod_data_source_block           compound5b
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4077102