Aqueous Chemistry of Chlorocyclophosphazenes: Phosphates {PO2}, Phosphamides {P(O)NHR}, and the first Phosphites {PHO} and Pyrophosphates {(PO)2O} of These Heterocycles
Joanne Ledger; Ramamoorthy Boomishankar; Alexander Steiner; Inorganic Chemistry 49 (2010) 3896–3904; doi:10.1021/ic100076t

data_4315322
_publ_section_title
;
 Aqueous Chemistry of Chlorocyclophosphazenes: Phosphates {PO2},
 Phosphamides {P(O)NHR}, and the first Phosphites {PHO} and Pyrophosphates
 {(PO)2O} of These Heterocycles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3896
_journal_page_last               3904
_journal_paper_doi               10.1021/ic100076t
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C24 H58 N7 O6 P3'
_chemical_formula_weight         633.68
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.251(2)
_cell_length_b                   19.868(4)
_cell_length_c                   29.263(6)
_cell_measurement_temperature    100(2)
_cell_volume                     6541(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Smart Apex'
_diffrn_measurement_method       /w
_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  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            32341
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6563
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.34(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         11486
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                9211
_reflns_number_total             11486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100076t_si_002_5.cif
_cod_data_source_block           jrl63a
_cod_database_code               4315322