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_4122394
_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_moiety
'4(C36 H30 N P2), Cr2 O24 P8, 0.70(C4 H10 O), 3.3(C2 H3 N)'
_chemical_formula_sum            'C153.41 H136.92 Cr2 N7.3 O24.7 P16'
_chemical_formula_weight         3077.45
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 96.5610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   9.1075(6)
_cell_length_b                   15.6495(10)
_cell_length_c                   24.7710(15)
_cell_measurement_reflns_used    9117
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      2.25
_cell_volume                     3507.4(4)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            113823
_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         30.037
_diffrn_reflns_theta_min         1.542
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1594
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         10266
_refine_ls_number_restraints     563
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0645P)^2^+3.6970P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7697
_reflns_number_total             10266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            5.cif
_cod_data_source_block           x13191
_cod_depositor_comments
'Adding full bibliography for 4122390--4122394.cif.'
_cod_original_formula_sum        'C153.41 H136.92 Cr2 N7.30 O24.70 P16'
_cod_database_code               4122394
_shelx_estimated_absorpt_t_min   0.900
_shelx_estimated_absorpt_t_max   0.980
_shelxl_version_number           2012-9
_shelx_res_checksum              5083
_shelx_hkl_checksum              39808