Electrophilic ring-opening of [(RP)nAs]− anions; a simple route to functionalised neutral phosphines of the type [(ButP)(ButRP)2]
Armstrong, David R.; Feeder, Neil; Hopkins, Alexander D.; Mays, Martin J.; Wood, Jody A.; Woods, Anthony D.; Wright, Dominic S.; Moncrieff, David; Chemical Communications  (2000) 2483–; doi:10.1039/b007553l

data_7111140
_publ_section_title
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 Electrophilic ring-opening of [(RP)nAs]&#x2212; anions; a simple route to
 functionalised neutral phosphines of the type [(ButP)(ButRP)2]
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_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2483
_journal_paper_doi               10.1039/b007553l
_journal_year                    2000
_chemical_formula_sum            'C16 H29 O4 P3 W'
_chemical_formula_weight         562.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3386(7)
_cell_length_b                   13.7599(5)
_cell_length_c                   9.4610(4)
_cell_measurement_temperature    180(2)
_cell_volume                     2257.18(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    teXsan
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            21678
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    5.345
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  1.156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
;
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.903
_refine_diff_density_min         -1.675
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.0011(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_all   1.076
_refine_ls_goodness_of_fit_obs   1.108
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2080
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.100
_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_obs          0.0267
_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^)+(0.0363P)^2^+1.2068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0664
_refine_ls_wR_factor_obs         0.0616
_reflns_number_observed          1790
_reflns_number_total             2087
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b007553lsup1.cif
_cod_data_source_block           dw9958
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'multiscan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+1.2068P] 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^)+(0.0363P)^2^+1.2068P] 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        2257.2(2)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7111140