Asymmetric Synthesis and Metal Complexes of aC3-Symmetric P-Stereogenic Triphosphine, (R)-MeSi(CH2PMe(t-Bu))3(MT-Siliphos)
Cain, Matthew F.; Glueck, David S.; Golen, James A.; Rheingold, Arnold L.; Organometallics 31 (2012) 775–; doi:10.1021/om200930k

data_4067934
_publ_section_title
;
 Asymmetric Synthesis and Metal Complexes of aC3-Symmetric P-Stereogenic
 Triphosphine, (R)-MeSi(CH2PMe(t-Bu))3(MT-Siliphos)
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              775
_journal_paper_doi               10.1021/om200930k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C27 H43 F6 N3 O6 P3 Ru S2 Si'
_chemical_formula_weight         905.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_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            16
_cell_length_a                   25.5296(15)
_cell_length_b                   25.5296(15)
_cell_length_c                   25.5296(15)
_cell_measurement_reflns_used    3975
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.72
_cell_measurement_theta_min      2.39
_cell_volume                     16639.2(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            72147
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7408
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_platon_squeeze_details
; 
 SQUEEZE (PLATON, A.Spek) was used to treat diffuse anion 
 contributions.  Total electron count found = 737/unit cell.  Calc.
 for 10.67 (2/3 x 16) triflate = 782/unit cell.  The intensive
 properties (density, F(000), etc.) reflect these contributions.  
;
_refine_diff_density_max         0.684
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         10183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+40.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1535
_reflns_number_gt                8765
_reflns_number_total             10183
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200930k_si_002.cif
_cod_data_source_block           glu375
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' 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_sg_symbol_H-M      P2(1)3
_cod_database_code               4067934