Rationally designed improvement of the bis(phospholano)ethane ligand for asymmetric hydrogenation leads to a reappraisal of the factors governing the enantioselectivity of Duphos catalysts
Fernandez, Elena; Gillon, Amy; Heslop, Katie; Horwood, Emily; Hyett, David J.; Orpen, A. Guy; Pringle, Paul G.; Chemical Communications  (2000) 1663–; doi:10.1039/b002994g

data_7115173
_publ_section_title
;
 Rationally designed improvement of the bis(phospholano)ethane ligand for
 asymmetric hydrogenation leads to a reappraisal of the factors governing
 the enantioselectivity of Duphos catalysts
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1663
_journal_paper_doi               10.1039/b002994g
_journal_year                    2000
_chemical_formula_sum            'C17 H32 I2 P2 Pt'
_chemical_formula_weight         747.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.699(3)
_cell_length_b                   12.699(2)
_cell_length_c                   11.995(2)
_cell_measurement_reflns_used    205
_cell_measurement_temperature    293(2)
_cell_volume                     1675.2(6)
_computing_cell_refinement       'SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SAINT (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement  'SHELXTL (Siemens, 1995a)'
_computing_structure_solution    'SHELXTL (Siemens, 1995a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation 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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11003
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    9.186
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.788110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
G M Sheldrick. SADABS: A program for absorption correction with the Siemens
SMART system; University of G\"ottingen: Germany,1996.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.222
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.626
_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                2331
_reflns_number_total             2589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002994g.txt
_cod_data_source_block           l-6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1675.1(5)
_cod_original_sg_symbol_H-M      P3(2)21
_cod_database_code               7115173