Structurally diverse penta- and hexacoordinate phosphorus compounds from the reaction of diethyl or diisopropyl azodicarboxylates with phosphorus(iii) compounds
Kumar, K. V. P. Pavan; Kumar, N. Satish; Kumara Swamy, K. C.; New Journal of Chemistry 30 (2006) 717–; doi:10.1039/b514839a

data_7052230
_publ_section_title
;
 Structurally diverse penta- and hexacoordinate phosphorus compounds
 from the reaction of diethyl or diisopropyl azodicarboxylates with
 phosphorus(iii) compounds
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              717
_journal_paper_doi               10.1039/b514839a
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C38 H50 N3 O6 P S'
_chemical_formula_weight         707.84
_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'
_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                 96.367(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.274(2)
_cell_length_b                   17.798(3)
_cell_length_c                   24.057(7)
_cell_measurement_temperature    293(2)
_cell_volume                     3946.3(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6872
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.9670
_exptl_absorpt_correction_T_min  0.9511
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1938
_reflns_number_gt                2968
_reflns_number_total             6872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b514839a.txt
_cod_data_source_block           compd17
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+0.0000P] 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^)+(0.0856P)^2^+0.0000P] 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        3946.2(16)
_cod_original_sg_symbol_H-M      p_21/n
_cod_database_code               7052230