Sterically Congested Tripodal Phosphites: Conformational Analysis, Solid-State Polymorphism, Metal Complexation, and Application to the Asymmetric Hydrosilation of Ketones1
Sai P. Shum; Stephen D. Pastor; Anthony D. DeBellis; Paul A. Odorisio; Lilibeth Burke; Frank H. Clarke; Grety Rihs; Bogdan Piatek; Ronald K. Rodebaugh; Inorganic Chemistry 42 (2003) 5097–5106; doi:10.1021/ic030099l

data_4314019
_publ_section_title
;
 Sterically Congested Tripodal Phosphites: Conformational Analysis,
 Solid-State Polymorphism, Metal Complexation, and Application to the
 Asymmetric Hydrosilation of Ketones1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5097
_journal_page_last               5106
_journal_paper_doi               10.1021/ic030099l
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C31 H46 N0.33 O3 P'
_chemical_formula_weight         502.32
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           146
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.000(10)
_cell_angle_beta                 90.000(10)
_cell_angle_gamma                120.000(10)
_cell_formula_units_Z            18
_cell_length_a                   25.991(3)
_cell_length_b                   25.991(3)
_cell_length_c                   24.649(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      20
_cell_volume                     14420(3)
_computing_cell_refinement       'CAD4 express'
_computing_data_collection       'CAD4 express'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18815
_diffrn_reflns_theta_max         69.96
_diffrn_reflns_theta_min         3.40
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.041
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4920
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.012
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.258
_refine_ls_goodness_of_fit_obs   1.282
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         9871
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.632
_refine_ls_restrained_S_obs      0.633
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_obs          0.0721
_refine_ls_shift/esd_max         -0.240
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1963
_refine_ls_wR_factor_obs         0.1621
_reflns_number_observed          7701
_reflns_number_total             11187
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic030099l_2.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        14420.3(29)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4314019