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_4078576
_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         'C41 H47 Ir O P2, 2(F6 Sb), C H2 Cl2'
_chemical_formula_sum            'C42 H49 Cl2 F12 Ir O P2 Sb2'
_chemical_formula_weight         1366.35
_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                 99.1190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.1907(7)
_cell_length_b                   12.8417(7)
_cell_length_c                   14.1613(8)
_cell_measurement_reflns_used    1838
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.56
_cell_measurement_theta_min      1.96
_cell_volume                     2368.5(2)
_computing_cell_refinement       'APEX2 v2008, Bruker AXS'
_computing_data_collection       'APEX2 v2008, Bruker AXS'
_computing_data_reduction        'APEX2 v2008, Bruker AXS'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.948
_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  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38771
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.56
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.195
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Numerical absorption correction based on indexing crystal faces, within
 APEX2 package were performed.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.158
_refine_diff_density_max         2.343
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         11150
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+2.9174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                11029
_reflns_number_total             11150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300346s_si_002.cif
_cod_data_source_block           compnd4
_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      P21
_cod_database_code               4078576