Oxyanion clusters with antielectrostatic hydrogen bonding (AEHB) in tetraalkylammonium hypodiphosphates
Emami, Marzieh; Ślepokura, Katarzyna Anna; Trzebiatowska, Monika; Noshiranzadeh, Nader; Kinzhybalo, Vasyl; CrystEngComm 20 (2018) 5209–; doi:10.1039/C8CE00880A

data_7231199
_publ_section_title
;
 Oxyanion clusters with antielectrostatic hydrogen bonding (AEHB) in
 tetraalkylammonium hypodiphosphates
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              5209
_journal_paper_doi               10.1039/C8CE00880A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety
'[(C8 H20 N), (H3 O6 P2)], 0.5(H4 O6 P2), 2(H2 O)'
_chemical_formula_sum            'C8 H29 N O11 P3'
_chemical_formula_weight         408.23
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-05-04 deposited with the CCDC.
2018-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                82.32(2)
_cell_angle_beta                 88.01(2)
_cell_angle_gamma                89.19(2)
_cell_formula_units_Z            12
_cell_length_a                   7.450(2)
_cell_length_b                   27.279(5)
_cell_length_c                   27.574(5)
_cell_measurement_reflns_used    27922
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      77.73
_cell_measurement_theta_min      1.62
_cell_volume                     5550(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 8.1956
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur PX, Onyx'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            81978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         77.942
_diffrn_reflns_theta_min         1.617
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.437
_exptl_absorpt_correction_T_max  0.701
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       plate
_exptl_crystal_F_000             2604
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.00061(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2015'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1334
_refine_ls_number_reflns         23476
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1163P)^2^+0.6347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.2005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15851
_reflns_number_total             23476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00880a2.cif
_cod_data_source_block           1_hyptet12ab
_cod_depositor_comments
'Adding full bibliography for 7231199--7231204.cif.'
_cod_database_code               7231199
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.278
_shelx_estimated_absorpt_t_max   0.704
_shelx_res_checksum              71272