The shortest C–H···O hydrogen bonds yet determined by single crystal neutron diffraction: a structural study of two phosphonium aryloxides
Matthew G. Davidson; Andrés E. Goeta; Judith A. K. Howard; Sarah Lamb; Sax A. Mason; New J. Chem. 24 (2000) 477–479; doi:10.1039/b001433h

data_7051283
_publ_section_title
;
 The shortest C--H&#x00B7;&#x00B7;&#x00B7;O hydrogen bonds yet
 determined by single crystal neutron diffraction: a structural study
 of two phosphonium aryloxides
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              477
_journal_page_last               479
_journal_paper_doi               10.1039/b001433h
_journal_volume                  24
_journal_year                    2000
_chemical_formula_sum            'C37 H31 O P'
_chemical_formula_weight         522.00
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                88.310(3)
_cell_angle_beta                 70.157(3)
_cell_angle_gamma                62.542(3)
_cell_formula_units_Z            4
_cell_length_a                   13.430(1)
_cell_length_b                   13.748(1)
_cell_length_c                   18.444(1)
_cell_measurement_reflns_used    5783
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      50.3
_cell_measurement_theta_min      3.1
_cell_volume                     2809.3(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      20(2)
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details
;  
D19 - ILL
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'Ge 115'
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.3137
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12265
_diffrn_reflns_theta_max         50.29
_diffrn_reflns_theta_min         2.20
_diffrn_source                   'nuclear reactor'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.7844
_exptl_absorpt_correction_T_min  0.4607
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             708
_exptl_crystal_size_max          4.9
_exptl_crystal_size_mid          3.9
_exptl_crystal_size_min          1.1
_refine_diff_density_max         0.853
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       0.00093(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.133
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1262
_refine_ls_number_reflns         8567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_obs          0.0440
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+25.6053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1319
_refine_ls_wR_factor_obs         0.1264
_reflns_number_observed          8018
_reflns_number_total             8567
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001433h.txt
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+25.6053P] 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^)+(0.0745P)^2^+25.6053P] 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        2809.2(1)
_cod_database_code               7051283