From light to heavy alkali metal tetraphosphonates (M = Li, Na, K, Rb, Cs): cation size-induced structural diversity and water-facilitated proton conductivity
Salcedo, Inés R.; Colodrero, Rosario M. P.; Bazaga-García, Montse; Vasileiou, Antonia; Papadaki, Maria; Olivera-Pastor, Pascual; Infantes-Molina, Antonia; Losilla, Enrique R.; Mezei, Gellert; Cabeza, Aurelio; Demadis, Konstantinos D.; CrystEngComm 20 (2018) 7648–; doi:10.1039/C8CE01351A

data_7235082
_publ_section_title
;
 From light to heavy alkali metal tetraphosphonates (M = Li, Na, K, Rb,
 Cs): cation size-induced structural diversity and water-facilitated
 proton conductivity
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              7648
_journal_paper_doi               10.1039/C8CE01351A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C10 H48 N2 Na2 O23 P4'
_chemical_formula_weight         734.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-11-09 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                97.3780(10)
_cell_angle_beta                 94.7920(10)
_cell_angle_gamma                101.7050(10)
_cell_formula_units_Z            2
_cell_length_a                   7.66820(10)
_cell_length_b                   11.53350(10)
_cell_length_c                   18.0768(2)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.29
_cell_volume                     1542.61(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74089
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.028
_diffrn_reflns_theta_min         1.824
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9784
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0404P)^2^+1.1108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7728
_reflns_number_total             9784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01351a2.cif
_cod_data_source_block           Na-HDTMP
_cod_database_code               7235082
_shelx_estimated_absorpt_t_min   0.854
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2014/6
_shelx_res_checksum              97284