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_7051284
_publ_section_title
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 The shortest C--H&#x00B7;&#x00B7;&#x00B7;O hydrogen bonds yet
 determined by single crystal neutron diffraction: a structural study
 of two phosphonium aryloxides
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_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            'C35 H43 O P'
_chemical_formula_weight         510.00
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.570(1)
_cell_length_b                   17.220(1)
_cell_length_c                   19.030(1)
_cell_measurement_reflns_used    3298
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      50.2
_cell_measurement_theta_min      3.5
_cell_volume                     6085.3(6)
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10445
_diffrn_reflns_theta_max         50.63
_diffrn_reflns_theta_min         3.58
_diffrn_source                   'nuclear reactor'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  0.5501
_exptl_absorpt_correction_T_min  0.3577
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          3.5
_exptl_crystal_size_mid          3.5
_exptl_crystal_size_min          2.4
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.00027(2)
_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_ref   1.171
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         4995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_obs          0.0357
_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^)+(0.0258P)^2^+19.6161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0738
_refine_ls_wR_factor_obs         0.0713
_reflns_number_observed          4467
_reflns_number_total             4995
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001433h.txt
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+19.6161P] 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^)+(0.0258P)^2^+19.6161P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7051284