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_4067932
_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 H53 F3 O3 P3 Rh S Si'
_chemical_formula_weight         738.66
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.046(2)
_cell_angle_beta                 74.7050(10)
_cell_angle_gamma                82.9590(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7734(3)
_cell_length_b                   11.6223(4)
_cell_length_c                   15.3027(5)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.20
_cell_measurement_theta_min      2.24
_cell_volume                     1664.01(9)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43204
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.24
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.9171
_exptl_absorpt_correction_T_min  0.7561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.025(10)
_refine_ls_extinction_coef       'not measured'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         20929
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0352P)^2^+0.7309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                20046
_reflns_number_total             20929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200930k_si_002.cif
_cod_data_source_block           glu371
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

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_sg_symbol_H-M      P1
_cod_database_code               4067932