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_4122390
_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 H60 N2 O11 P8'
_chemical_formula_weight         1376.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.2850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4891(13)
_cell_length_b                   15.2366(11)
_cell_length_c                   25.1850(18)
_cell_measurement_temperature    100(2)
_cell_volume                     6503.7(8)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            183927
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         1.201
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.9619
_exptl_absorpt_correction_T_min  0.9309
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         19837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0515P)^2^+4.0680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15509
_reflns_number_total             19837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2.cif
_cod_data_source_block           13013
_cod_depositor_comments
'Adding full bibliography for 4122390--4122394.cif.'
_cod_original_cell_volume        6503.6(8)
_cod_database_code               4122390
_shelx_estimated_absorpt_t_min   0.931
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2013-4
_shelx_res_checksum              9022
_shelx_hkl_checksum              5707