Metal Complexes of <i>trans</i>-2,2,4,4-Tetrafluoro-1,3-di-<i>tert</i>-butyl-1,3-diphosphetane
Jones, P. G.; Thöne, C.; Acta Crystallographica Section C 53 (1997) 42–45; doi:10.1107/S0108270196011870

data_2005849
_publ_section_title
;
 Metal Complexes of
 <i>trans</i>-2,2,4,4-Tetrafluoro-1,3-di-<i>tert</i>-butyl-1,3-diphosphetane
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              42
_journal_page_last               45
_journal_paper_doi               10.1107/S0108270196011870
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[W (C10 H18 F4 P2) (C O)5]'
_chemical_formula_sum            'C15 H18 F4 O5 P2 W'
_chemical_formula_weight         600.08
_chemical_name_systematic
;
 {trans-(2,2,4,4-tetrafluoro-1,3-di-t-butyl-1,3-diphosphetane)}-
 pentacarbonyltungsten(0)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.79(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.505(4)
_cell_length_b                   11.657(3)
_cell_length_c                   21.918(6)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      10
_cell_volume                     4155.6(19)
_computing_cell_refinement       P3
_computing_data_collection       'P3 (Nicolet, 1987)'
_computing_data_reduction        'XSCANS (Siemens, 1994b)'
_computing_molecular_graphics    'XP (Siemens, 1994a)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      178(2)
_diffrn_measurement_device       'Siemens R3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8812
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.770
_exptl_absorpt_correction_T_max  0.315
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_type   '\y scans (XEMP; Siemens, 1990)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.105
_refine_diff_density_min         -0.745
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.993
_refine_ls_goodness_of_fit_obs   1.037
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         7283
_refine_ls_number_restraints     278
_refine_ls_restrained_S_all      0.979
_refine_ls_restrained_S_obs      1.015
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_obs          0.0306
_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^)+(0.0405P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0786
_refine_ls_wR_factor_obs         0.0677
_reflns_number_observed          5113
_reflns_number_total             7283
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bs1001.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (32
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (44 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0405P)^2^] 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^)+(0.0405P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2005849