Gallium Halide Induced Heterocycle Expansion of Dihalodiphosphadiaryldiazanes [(XPNR)2] to the Corresponding Triphosphatriazanes [(XPNR)3]
Neil Burford; Korey D. Conroy; Jeff C. Landry; Paul J. Ragogna; Michael J. Ferguson; Robert McDonald; Inorganic Chemistry 43 (2004) 8245–8251; doi:10.1021/ic049217a

data_4312277
_publ_section_title
;
 Gallium Halide Induced Heterocycle Expansion of
 Dihalodiphosphadiaryldiazanes [(XPNR)2] to the Corresponding
 Triphosphatriazanes [(XPNR)3]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8245
_journal_page_last               8251
_journal_paper_doi               10.1021/ic049217a
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C16 H18 Cl2 N2 P2'
_chemical_formula_sum            'C16 H18 Cl2 N2 P2'
_chemical_formula_weight         371.16
_chemical_melting_point          394(2)
_chemical_name_common            '[DmpNPCl]2'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 105.6520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2850(7)
_cell_length_b                   11.2343(7)
_cell_length_c                   14.3926(8)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.392
_cell_measurement_theta_min      2.334
_cell_volume                     1757.02(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8956
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.05
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.8935
_exptl_absorpt_correction_T_min  0.7560
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   emperical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+4.1275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                3199
_reflns_number_total             3564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049217asi20040616_025301_1.cif
_cod_data_source_block           dal0241
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '392-396' was changed to '394(2)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_database_code               4312277