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_7235081
_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 H34 Li2 N2 O16 P4'
_chemical_formula_weight         576.15
_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                74.418(7)
_cell_angle_beta                 76.170(7)
_cell_angle_gamma                84.313(7)
_cell_formula_units_Z            1
_cell_length_a                   5.9728(6)
_cell_length_b                   9.4557(9)
_cell_length_c                   11.0182(11)
_cell_measurement_reflns_used    1719
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.64
_cell_measurement_theta_min      2.58
_cell_volume                     581.62(10)
_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 0.991
_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  0.0800
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10054
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.569
_diffrn_reflns_theta_min         1.968
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  0.9841
_exptl_absorpt_correction_T_min  0.9167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       prism
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2408
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1018P)^2^+0.0500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1693
_reflns_number_total             2408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01351a2.cif
_cod_data_source_block           Li-HDTMP
_cod_database_code               7235081
_shelx_estimated_absorpt_t_min   0.917
_shelx_estimated_absorpt_t_max   0.984
_shelxl_version_number           2014/6
_shelx_res_checksum              3646