A Triphenylphoshine Oxide-Water Aggregate Facilitates an Exceptionally Short C-H...O Hydrogen Bond
Benson M. Kariuki; Kenneth D. M. Harris; Douglas Philp; James M. A. Robinson; Journal of the American Chemical Society 119 (1997) 12679–12680; doi:10.1021/ja973506z

data_4117099
_publ_section_title
;
 A Triphenylphoshine Oxide-Water Aggregate Facilitates an Exceptionally
 Short C-H...O Hydrogen Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12679
_journal_page_last               12680
_journal_paper_doi               10.1021/ja973506z
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C82 H70 O6 P4'
_chemical_formula_weight         1275.26
_chemical_name_common
'Tetrakis(triphenylphosphine oxide)-diethynylbenzene-bis(water) clathrate'
_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                101.143(3)
_cell_angle_beta                 102.256(4)
_cell_angle_gamma                86.064(2)
_cell_formula_units_Z            1
_cell_length_a                   9.7929(8)
_cell_length_b                   20.9698(15)
_cell_length_c                   8.8836(6)
_cell_measurement_reflns_used    5311
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      1.41
_cell_volume                     1748.4(2)
_computing_cell_refinement       'R-Axis II software (Rigaku Corporation,1994)'
_computing_data_collection       'R-Axis II software (Rigaku Corporation,1994)'
_computing_data_reduction        'TEXSAN (Molecular Structure Corporation,1993)'
_computing_publication_material  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'TEXSAN (Molecular Structure Corporation,1993)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'Rigaku R-Axis II area detector'
_diffrn_measurement_method       'Image plate scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10456
_diffrn_reflns_theta_max         25.18
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       'Transparent plates'
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.028
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.126
_refine_ls_goodness_of_fit_obs   1.135
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_restrained_S_obs      1.135
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_obs          0.0480
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.4925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1141
_refine_ls_wR_factor_obs         0.1115
_reflns_number_observed          5311
_reflns_number_total             5626
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja973506z.cif
_cod_data_source_block           TPPO_diethynylbenzene_hydrate
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.4925P] 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^)+(0.0374P)^2^+0.4925P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4117099