Enantioselective Catalytic Diels‒Alder Reactions with Enones As Dienophiles
Carmona, Daniel; Viguri, Fernando; Asenjo, Ainara; Lahoz, Fernando J.; García-Orduña, Pilar; Oro, Luis A.; Organometallics 31 (2012) 4551–; doi:10.1021/om300346s

data_4078577
_publ_section_title
;
 Enantioselective Catalytic Diels--Alder Reactions with Enones As
 Dienophiles
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              4551
_journal_paper_doi               10.1021/om300346s
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C42 H49 Ir O P2, 2(F6 Sb), C H2 Cl2'
_chemical_formula_sum            'C43 H51 Cl2 F12 Ir O P2 Sb2'
_chemical_formula_weight         1380.38
_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                 96.429(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.132(4)
_cell_length_b                   13.166(4)
_cell_length_c                   14.039(5)
_cell_measurement_reflns_used    1129
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.875
_cell_measurement_theta_min      2.253
_cell_volume                     2412.0(13)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD sysyem'
_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  0.0913
_diffrn_reflns_av_sigmaI/netI    0.1310
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13405
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.120
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.45.                    
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.023
_refine_diff_density_max         3.264
_refine_diff_density_min         -2.178
_refine_diff_density_rms         0.249
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6380
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0723P)^2^+11.0310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1758
_reflns_number_gt                4329
_reflns_number_total             6380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300346s_si_002.cif
_cod_data_source_block           compnd5
_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_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4078577