Crystalline Metaphosphate Acid Salts: Synthesis in Organic Media, Structures, Hydrogen-Bonding Capability, and Implication of Superacidity.
Chakarawet, Khetpakorn; Knopf, Ioana; Nava, Matthew; Jiang, Yanfeng; Stauber, Julia M.; Cummins, Christopher C.; Inorganic chemistry 55 (2016) 6178–6185; doi:10.1021/acs.inorgchem.6b00749

data_4347880
_publ_section_title
;
 Crystalline Metaphosphate Acid Salts: Synthesis in Organic Media,
 Structures, Hydrogen-Bonding Capability, and Implication of Superacidity.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6178
_journal_page_last               6185
_journal_paper_doi               10.1021/acs.inorgchem.6b00749
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C76 H69 N2 O10 P7'
_chemical_formula_weight         1387.12
_chemical_name_systematic
'Bis(triphenylphosphine)iminium hydrogentrimetaphosphate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 102.843(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5931(13)
_cell_length_b                   25.176(3)
_cell_length_c                   12.9215(15)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.49
_cell_measurement_theta_min      2.29
_cell_volume                     3359.8(7)
_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-2013 (Sheldrick, 2013)'
_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 0.986
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            113001
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.529
_diffrn_reflns_theta_min         1.616
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.7147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.41(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     906
_refine_ls_number_reflns         21387
_refine_ls_number_restraints     2040
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0488P)^2^+1.1066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                20609
_reflns_number_total             21387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00749_si_003.cif
_cod_data_source_block           x8_14028
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4347880
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.939
_shelxl_version_number           2013-4
_shelx_res_checksum              38075
_shelx_hkl_checksum              97658