Enantioselective Catalysts for the Diels‒Alder Reaction between Methacrolein and Cyclopentadiene Based on the Chiral Fragment (η5-C5Me5)M(chiral diphosphane) (M = Rh, Ir)
Carmona, Daniel; Viguri, Fernando; Asenjo, Ainara; Lamata, M. Pilar; Lahoz, Fernando; Garc\?ía-Orduña, Pilar; Oro, L. A.; Organometallics 30 (2011) 6661–; doi:10.1021/om200859z

data_4065499
_publ_section_title
;
 Enantioselective Catalysts for the Diels--Alder Reaction between
 Methacrolein and Cyclopentadiene Based on the Chiral Fragment
 (\h5-C5Me5)M(chiral diphosphane) (M = Rh, Ir)
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6661
_journal_paper_doi               10.1021/om200859z
_journal_volume                  30
_journal_year                    2011
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C47 H51 O P2 Rh, 2(F6 Sb), 2(C6 H14)'
_chemical_formula_sum            'C59 H79 F12 O P2 Rh Sb2'
_chemical_formula_weight         1440.57
_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                   11.1778(14)
_cell_length_b                   15.922(2)
_cell_length_c                   30.769(4)
_cell_measurement_reflns_used    5473
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.607
_cell_measurement_theta_min      2.226
_cell_volume                     5476.0(12)
_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    'DIRDIF (Beurskens, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0713
_diffrn_reflns_av_sigmaI/netI    0.0963
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            31927
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package.                    
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 The unit cell contains 12 hexane molecules which have been treated as a 
 diffuse contribution to the overall scattering without specific atom positions
 by SQUEEZE/PLATON
;
_refine_diff_density_max         2.031
_refine_diff_density_min         -1.581
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(34)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         11188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0977P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1749
_reflns_number_gt                7497
_reflns_number_total             11188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200859z_si_002.cif
_cod_data_source_block           comp13
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5476.1(12)
_cod_database_code               4065499