Oxidative Addition of Tetrachloro-1,2-benzoquinone to λ3-Cyclotriphosphazanes. An Unusual Ring Contraction-Rearrangement
Natesan Thirupathi; Setharampattu S. Krishnamurthy; Munirathinam Nethaji; Inorganic Chemistry 38 (1999) 1093–1098; doi:10.1021/ic980459i

data_4321821
_publ_section_title
;
 Oxidative Addition of Tetrachloro-1,2-benzoquinone to
 \l3-Cyclotriphosphazanes. An Unusual Ring Contraction-Rearrangement
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1093
_journal_page_last               1098
_journal_paper_doi               10.1021/ic980459i
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesis
_chemical_formula_sum            'C40 H37 Br Cl8 N3 O7 P3'
_chemical_formula_weight         1128.15
_chemical_melting_point          583
_chemical_name_common            \5-Cyclodiphosphazanes
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                87.19(2)
_cell_angle_beta                 73.42(1)
_cell_angle_gamma                80.47(1)
_cell_formula_units_Z            2
_cell_length_a                   11.027(1)
_cell_length_b                   14.226(4)
_cell_length_c                   16.143(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      8
_cell_volume                     2393.6(8)
_computing_cell_refinement       'Enraf-Nonius CAD-4 Diffractometer'
_computing_data_collection       'Enraf-Nonius CAD-4 Diffractometer'
_computing_data_reduction        local
_computing_molecular_graphics    'ORTEP II'
_computing_publication_material  CIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 Diffractometer'
_diffrn_measurement_method       'w-2theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_sigmaI/netI    0.0957
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8952
_diffrn_reflns_theta_max         31.21
_diffrn_reflns_theta_min         1.32
_diffrn_standards_interval_count 400
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_T_max  1.131
_exptl_absorpt_correction_T_min  0.999
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         .280
_refine_diff_density_min         -.651
_refine_diff_density_rms         .064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.130
_refine_ls_goodness_of_fit_obs   1.243
_refine_ls_hydrogen_treatment    constraint
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         8388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_restrained_S_obs      1.243
_refine_ls_R_factor_all          0.1929
_refine_ls_R_factor_obs          0.0784
_refine_ls_shift/esd_max         0.318
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0508P)^2^+4.7281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1934
_refine_ls_wR_factor_obs         0.1369
_reflns_number_observed          3779
_reflns_number_total             8398
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980459i.cif
_cod_data_source_block           5het
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0508P)^2^+4.7281P] 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^)+( 0.0508P)^2^+4.7281P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321821