Chiral Octahedral Phosphano‒Oxazoline Iridium(III) Complexes as Catalysts in Asymmetric Cycloaddition Reactions
Carmona, Daniel; Ferrer, Joaquina; Garc\?ía, Néstor; Ram\?írez, Paola; Lahoz, Fernando J.; Garc\?ía-Orduña, Pilar; Oro, Luis A.; Organometallics 32 (2013) 1609–; doi:10.1021/om301089c

data_4080337
_publ_section_title
;
 Chiral Octahedral Phosphano--Oxazoline Iridium(III) Complexes as
 Catalysts in Asymmetric Cycloaddition Reactions
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1609
_journal_paper_doi               10.1021/om301089c
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C54 H49 Ir N O2 P3, 2(F6 Sb), 2 (C4 H10 O), H2 O'
_chemical_formula_sum            'C62 H71 F12 Ir N O5 P3 Sb2'
_chemical_formula_weight         1666.81
_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                 94.5270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.6736(8)
_cell_length_b                   23.6185(17)
_cell_length_c                   11.8942(8)
_cell_measurement_reflns_used    2701
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.22
_cell_measurement_theta_min      2.35
_cell_volume                     3269.2(4)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10,Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.10,BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.1004
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25174
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    3.006
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.01.                    
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.077
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.009
_refine_diff_density_max         2.107
_refine_diff_density_min         -1.433
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         14045
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0448P)^2^+0.0787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                11624
_reflns_number_total             14045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301089c_si_002.cif
_cod_data_source_block           cmpnd_1
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4080337