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_4080340
_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
'2(C60 H57 Ir N O2 P3), 4(F6 Sb),C H2 Cl2,3(C6 H14)'
_chemical_formula_sum            'C139 H158 Cl2 F24 Ir2 N2 O4 P6 Sb4'
_chemical_formula_weight         3504.98
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 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            4
_cell_length_a                   25.703(3)
_cell_length_b                   26.433(3)
_cell_length_c                   21.329(2)
_cell_measurement_reflns_used    5254
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.948
_cell_measurement_theta_min      2.206
_cell_volume                     14491(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX CCD system'
_diffrn_measurement_method       'narrow \w 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  0.1072
_diffrn_reflns_av_sigmaI/netI    0.0860
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            68844
_diffrn_reflns_theta_full        20.14
_diffrn_reflns_theta_max         20.14
_diffrn_reflns_theta_min         1.23
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.749
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package.                    
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             6944
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.058
_platon_squeeze_details
;
 The total potential solvent accesible void volume (2275 \A3)  and 
 the electron count  (762 e in the unit cell) may agree with the 
 presence of twelve n-hexane molecules  (C6 H14). They have been 
 included in the chemical formula, F00 and density. 
;
_refine_diff_density_max         1.871
_refine_diff_density_min         -2.008
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.057(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         13738
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1401P)^2^+139.7014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2308
_refine_ls_wR_factor_ref         0.2468
_reflns_number_gt                10041
_reflns_number_total             13738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301089c_si_002.cif
_cod_data_source_block           cmpnd_11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        14491(2)
_cod_original_sg_symbol_H-M      P21212
_cod_database_code               4080340