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_4312279
_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 Br2 N2 P2'
_chemical_formula_sum            'C16 H18 Br2 N2 P2'
_chemical_formula_weight         460.08
_chemical_melting_point          501(2)
_chemical_name_common            '[DmpNPBr]2'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.628(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.7724(16)
_cell_length_b                   11.5131(12)
_cell_length_c                   20.513(2)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.322
_cell_measurement_theta_min      2.216
_cell_volume                     3604.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15765
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.33
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.673
_exptl_absorpt_correction_T_max  0.2565
_exptl_absorpt_correction_T_min  0.1384
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   emperical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         7334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+1.1041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                5374
_reflns_number_total             7334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049217asi20040616_025301_3.cif
_cod_data_source_block           dal0301
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '499-503' was changed to '501(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_original_cell_volume        3604.3(6)
_cod_database_code               4312279