Dihydrogen Tetrametaphosphate, [P4O12H2](2-): Synthesis, Solubilization in Organic Media, Preparation of its Anhydride [P4O11](2-) and Acidic Methyl Ester, and Conversion to Tetrametaphosphate Metal Complexes via Protonolysis.
Jiang, Yanfeng; Chakarawet, Khetpakorn; Kohout, Andrea Laura; Nava, Matthew; Marino, Nadia; Cummins, Christopher C.; Journal of the American Chemical Society 136 (2014) 11894–11897; doi:10.1021/ja5058339

data_4122393
_publ_section_title
;
 Dihydrogen Tetrametaphosphate, [P4O12H2](2-): Synthesis, Solubilization
 in Organic Media, Preparation of its Anhydride [P4O11](2-) and Acidic
 Methyl Ester, and Conversion to Tetrametaphosphate Metal Complexes via
 Protonolysis.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11894
_journal_page_last               11897
_journal_paper_doi               10.1021/ja5058339
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C72 H62 N2 O12 P8'
_chemical_formula_weight         1394.99
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9148(9)
_cell_length_b                   16.3924(7)
_cell_length_c                   19.9502(9)
_cell_measurement_temperature    100(2)
_cell_volume                     6512.8(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            75134
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.579
_diffrn_reflns_theta_min         1.906
_exptl_absorpt_coefficient_mu    0.281
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         9957
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+3.8045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8381
_reflns_number_total             9957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           x813135
_cod_depositor_comments
'Adding full bibliography for 4122390--4122394.cif.'
_cod_database_code               4122393
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.920
_shelxl_version_number           2013-4
_shelx_res_checksum              52998
_shelx_hkl_checksum              26420