Different thermal reactivity of a 1,2-thiaphospholo[a]phosphirane in free and metal carbonyl complexed form
Jikyo, Tamaki; Maas, Gerhard; Chemical Communications (Cambridge, United Kingdom)  (2003) 2794–2795; doi:10.1039/b310256d

data_7113469
_publ_section_title
;
 Different thermal reactivity of a 1,2-thiaphospholo[a]phosphirane in free
 and metal carbonyl complexed form
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   22
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2794
_journal_page_last               2795
_journal_paper_doi               10.1039/b310256d
_journal_year                    2003
_chemical_formula_moiety         (C28H21PS)xW(CO)5
_chemical_formula_sum            'C33 H21 O5 P S W'
_chemical_formula_weight         744.38
_chemical_melting_point          446.6(5)
_chemical_name_common
;
2,3a,8-triphenyl-3a,8-dihydro-1-thia-8a-
phosphacyclopenta(a)indene P-(pentacarbonyl)tungsten
;
_chemical_name_systematic
;
2,3a,8-triphenyl-3a,8-dihydro-1-thia-8a-phosphacyclopenta[a]indene
P-(pentacarbonyl)tungsten
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.81(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8753(16)
_cell_length_b                   10.701(2)
_cell_length_c                   30.832(5)
_cell_measurement_temperature    193(2)
_cell_volume                     2924.7(9)
_computing_cell_refinement       'IPDS software (Stoe, Darmstadt)'
_computing_data_collection       'IPDS software (Stoe, Darmstadt)'
_computing_data_reduction        'X-RED (Stoe, Darmstadt)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1998)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'IPDS (Stoe, Darmstadt)'
_diffrn_measurement_method       'Phi scans, rotation mode'
_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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            20349
_diffrn_reflns_theta_full        24.06
_diffrn_reflns_theta_max         24.06
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    4.116
_exptl_absorpt_correction_T_max  0.6600
_exptl_absorpt_correction_T_min  0.1900
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         4431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                3209
_reflns_number_total             4431
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7104903
_cod_data_source_file            b310256d.txt
_cod_data_source_block           jik020
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '173-174 \%C' was changed to
'446.6(5)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               7113469