Synthesis of novel axially chiral Rh?NHC complexes derived from BINAM and application in the enantioselective hydrosilylation of methyl ketonesElectronic supplementary information (ESI) available: 13C NMR and 1H NMR spectral and analytic data for compounds 2?7, reduction products, and chiral HPLC and GC charts for sec-alcohols 9a?m. See http://www.rsc.org/suppdata/cc/b3/b309185f/
Duan, Wei-Liang; Shi, Min; Rong, Guo-Bin; Chemical Communications  (2003) 2916–; doi:10.1039/b309185f

data_7111303
_publ_section_title
;
 Synthesis of novel axially chiral Rh?NHC complexes derived from BINAM and
 application in the enantioselective hydrosilylation of methyl
 ketonesElectronic supplementary information (ESI) available: 13C NMR and
 1H NMR spectral and analytic data for compounds 2?7, reduction products,
 and chiral HPLC and GC charts for sec-alcohols 9a?m. See
 http://www.rsc.org/suppdata/cc/b3/b309185f/
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2916
_journal_paper_doi               10.1039/b309185f
_journal_year                    2003
_chemical_formula_sum            'C40 H33 I2 N4 O2.5 Rh'
_chemical_formula_weight         966.41
_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            8
_cell_length_a                   17.4433(9)
_cell_length_b                   17.9331(9)
_cell_length_c                   27.9530(14)
_cell_measurement_reflns_used    4371
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.545
_cell_measurement_theta_min      4.771
_cell_volume                     8744.0(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1202
_diffrn_reflns_av_sigmaI/netI    0.2273
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            53351
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.838
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83825
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.720
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_coef       0.00063(7)
_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   0.834
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         20291
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.835
_refine_ls_R_factor_all          0.1872
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.383
_refine_ls_shift/su_mean         0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1940
_reflns_number_gt                7436
_reflns_number_total             20291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b309185fsup1.cif
_cod_data_source_block           cd2386
_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_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_original_formula_sum        'C40 H33  N4 O2.50 I2 Rh'
_cod_database_code               7111303