Synthesis of η^4^:π^2^-Exocyclic-Diene Iridium(I) Complexes Derived from 1,3-Oxazolidin-2-ones and Their Transformation into Iridium(III) Derivatives by Reaction with a Phosphine and with Aldehydes
Salazar, Verónica; Suárez-Castillo, Oscar R.; Padilla, Rosa; Macías Pulido, Juan Carlos; Méndez-Rojas, Miguel Ángel; Tamariz, Joaquín; Benavides, Adriana; Organometallics 25 (2006) 172–176; doi:10.1021/om050582z

data_4060582
_publ_section_title
;
Synthesis of \h^4^:\p^2^-Exocyclic-Diene Iridium(I) Complexes Derived from 
1,3-Oxazolidin-2-ones and Their Transformation into Iridium(III) 
Derivatives by Reaction with a Phosphine and with Aldehydes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              172
_journal_page_last               176
_journal_paper_doi               10.1021/om050582z
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C33 H39 B Ir N7 O2'
_chemical_formula_sum            'C35 H45 B Ir N7 O3'
_chemical_formula_weight         814.79
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.93(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.707(7)
_cell_length_b                   26.84(3)
_cell_length_c                   14.283(7)
_cell_measurement_temperature    293(2)
_cell_volume                     3540(5)
_computing_cell_refinement       'SAINT+ v. 7.06 a (Bruker AXS, 2003)'
_computing_data_collection       'APEX-W2K-NT v. 1.0 (Bruker AXS, 2004)'
_computing_data_reduction        'SAINT+ v. 7.06 a (Bruker AXS, 2001)'
_computing_molecular_graphics    'XP, SXGRAPH v. 6.10 (WinGX)'
_computing_publication_material  'XCIF, SHELXTL v. 6.10 (WinGX)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(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-Nonius SMART 5000 CCD'
_diffrn_measurement_method       'omega scans 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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23256
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.52
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    3.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS: Area-Detector Absorption Correction. Bruker-AXS within 
v. 7.06 a (Bruker AXS, 2003).
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.507
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.00085(10)
_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   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                5471
_reflns_number_total             6940
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4060582