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_4314018
_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            'C90 H132 N O9 P3'
_chemical_formula_weight         1464.88
_space_group_IT_number           2
_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
_cell_angle_alpha                116.230(10)
_cell_angle_beta                 100.150(10)
_cell_angle_gamma                91.070(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4930(10)
_cell_length_b                   19.701(2)
_cell_length_c                   21.027(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35
_cell_measurement_theta_min      25
_cell_volume                     4542.3(9)
_computing_cell_refinement       cad4
_computing_data_collection       cad4
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -1
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_diffrn_standards_decay_%        2
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_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_description       cube
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.603
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_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    riding
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_refine_ls_R_factor_obs          0.0748
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_refine_ls_shift/esd_mean        0.036
_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         0.2398
_refine_ls_wR_factor_obs         0.2330
_reflns_number_observed          8103
_reflns_number_total             9336
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic030099l_1.cif
_cod_data_source_block           artm
_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        4542.3(7)
_cod_database_code               4314018