1,2,3-triphosphole derivatives as reactive intermediates.
Stubenhofer, Markus; Kuntz, Christian; Balázs, Gábor; Zabel, Manfred; Scheer, Manfred; Chemical communications (Cambridge, England) 34 (2009) 1745–1747; doi:10.1039/b822732b

data_7104288
_publ_section_title
;
 1,2,3-triphosphole derivatives as reactive intermediates.
;
_journal_issue                   13
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1745
_journal_page_last               1747
_journal_paper_doi               10.1039/b822732b
_journal_volume                  34
_journal_year                    2009
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C32 H10 O20 P6 W4, C H2 Cl2'
_chemical_formula_sum            'C33 H12 Cl2 O20 P6 W4'
_chemical_formula_weight         1720.51
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                111.295(6)
_cell_angle_beta                 104.846(7)
_cell_angle_gamma                99.201(18)
_cell_formula_units_Z            2
_cell_length_a                   11.547(3)
_cell_length_b                   14.237(3)
_cell_length_c                   17.070(7)
_cell_measurement_reflns_used    6178
_cell_measurement_temperature    123
_cell_measurement_theta_max      62.1439
_cell_measurement_theta_min      2.9566
_cell_volume                     2425.6(13)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1993)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.790
_diffrn_measured_fraction_theta_max 0.790
_diffrn_measurement_details
;
1 omega -27.00 22.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -1.2571 45.0000 120.0000 0.0000 0.0000 49

2 omega -21.00 26.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 2.5071 45.0000 240.0000 0.0000 0.0000 47

3 phi -177.00 -119.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
40.0000 2.5071 0.0000 - 0.0000 0.0000 58

4 omega -113.00 -57.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 106.0000 227.0000 0.0000 0.0000 56

5 phi -31.00 31.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
-40.0000 -83.1433 0.0000 - 0.0000 0.0000 62

6 omega -115.00 -59.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 75.0000 0.0000 0.0000 0.0000 56

7 omega -107.00 -50.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 -79.0000 314.0000 0.0000 0.0000 57

8 omega -107.00 -56.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 -45.0000 240.0000 0.0000 0.0000 51

9 omega -115.00 -61.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 112.0000 60.0000 0.0000 0.0000 54

10 omega 54.00 82.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 84.3933 -121.0000 217.0000 0.0000 0.0000 28

11 omega 81.00 109.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 84.3933 -45.0000 120.0000 0.0000 0.0000 28

12 omega 58.00 109.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 84.3933 45.0000 0.0000 0.0000 0.0000 51

13 omega 11.00 61.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 84.3933 -45.0000 120.0000 0.0000 0.0000 50

14 omega 60.00 100.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 84.3933 -45.0000 0.0000 0.0000 0.0000 40

15 omega 105.00 133.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 84.3933 64.0000 -48.0000 0.0000 0.0000 28

;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10270
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        62.12
_diffrn_reflns_theta_max         62.12
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    20.615
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.356
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       'flat prism'
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
With the aid of PLATON two solvent accessible areas were found, but it was
impossible to refine any reasonable molecule from difference Fourier peaks.
Therefore the midpoint, the size and the number of electrons in these voids
were refined and the contribution to the calculated structure factors of
the disordered solvent is taken into account by back-Fourier transformation
with the program SQUEEZE (Sluis and Spek, 1990). The void were found at
(0.500, 1.000, 0.500 ) the sizes is 96\%A^3^, 38 e^-^. This electron
number corresponds to one dichlormethane molecule.
;
_refine_diff_density_max         1.270
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         6061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                4743
_reflns_number_total             6061
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b822732b.txt
_cod_data_source_block           pw2ph
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               7104288