Diastereoselective Synthesis of Chiral Octahedral Iridium(III) Phosphano‒Oxazoline Complexes
Carmona, Daniel; Ferrer, Joaquina; Garc\?ía, Néstor; Ramírez, Paola; Lahoz, Fernando J.; Garc\?ía-Orduña, Pilar; Oro, Luis A.; Organometallics 32 (2013) 1595–; doi:10.1021/om301088x

data_4080336
_publ_section_title
;
 Diastereoselective Synthesis of Chiral Octahedral Iridium(III)
 Phosphano--Oxazoline Complexes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1595
_journal_paper_doi               10.1021/om301088x
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C50 H28 F20 Ir N O P3, Sb F6'
_chemical_formula_sum            'C50 H28 F26 Ir N O P3 Sb'
_chemical_formula_weight         1559.59
_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                   11.1488(7)
_cell_length_b                   21.9003(14)
_cell_length_c                   22.0481(15)
_cell_measurement_reflns_used    1741
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.78
_cell_measurement_theta_min      2.25
_cell_volume                     5383.3(6)
_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 v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, 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  0.1050
_diffrn_reflns_av_sigmaI/netI    0.1265
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29726
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.190
_exptl_absorpt_correction_T_max  0.7984
_exptl_absorpt_correction_T_min  0.4125
_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            orange
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.283
_refine_diff_density_min         -1.681
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         9500
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+19.0665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1828
_reflns_number_gt                6648
_reflns_number_total             9500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301088x_si_001.cif
_cod_data_source_block           cmpnd_18
_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_database_code               4080336