Solving the P-O/P-OH riddle: direct synthesis and neutron diffraction characterization of dianionic dithiophosphonates.
Pillay, Michael N.; Li, Min-Chi; Ni, Yu-Rong; Yen, Wei-Jung; Chiu, Tzu-Hao; Wang, Xiaoping; Saillard, Jean-Yves; Liu, C. W.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 1637–1641; doi:10.1039/d5dt02816g

data_7720452
_publ_section_title
;
 Solving the P-O/P-OH riddle: direct synthesis and neutron diffraction
 characterization of dianionic dithiophosphonates.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1637
_journal_page_last               1641
_journal_paper_doi               10.1039/d5dt02816g
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C14 H14 Ni O4 P2 S4, H2 O, 2(H4 N)'
_chemical_formula_sum            'C14 H24 N2 Ni O5 P2 S4'
_chemical_formula_weight         549.24
_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'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-11-09 deposited with the CCDC.	2025-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.2810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3772(3)
_cell_length_b                   10.46930(10)
_cell_length_c                   14.2568(2)
_cell_measurement_reflns_used    21937
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      78.228
_cell_measurement_theta_min      7.443
_cell_volume                     2261.93(6)
_computing_cell_refinement       'TOPAZ Mantid Python Program'
_computing_data_collection       'SNS EPICS'
_computing_data_reduction        'TOPAZ Mantid Python Program'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  TOPAZ
_diffrn_measurement_method       'time-of-flight Laue'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.00
_diffrn_radiation_wavelength_details 'Based on neutron time of flight'
_diffrn_reflns_av_R_equivalents  0.1848
_diffrn_reflns_av_unetI/netI     0.1113
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58323
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        36.870
_diffrn_reflns_theta_max         78.263
_diffrn_reflns_theta_min         7.400
_diffrn_source                   'The ORNL Spallation Neutron Source'
_exptl_absorpt_coefficient_mu    0.1758
_exptl_absorpt_correction_T_max  0.8879
_exptl_absorpt_correction_T_min  0.7039
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
; 
C. W. Dwiggins, Jr., Acta Cryst. A31, 395 (1975).
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          1.200
_exptl_crystal_size_mid          1.100
_exptl_crystal_size_min          0.850
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       0.00375(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0172P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5967
_reflns_number_total             8404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02816g2.cif
_cod_data_source_block           NiAq_neutron
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7720452
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.972
_exptl_absorpt_special_details
; 
Neutron linear absorption coefficient is wavelength dependent.
For each peak, the absorption coefficient mu is calculated as:
          mu = 1.0200 + 1.3270/1.7982 * wavelength  [cm^-1^]
where 
 1.0200 cm^-1 is the absorption coefficient for total scattering;
 1.3270 cm^-1 is the absorption coefficient for true absorption at 1.7982 A.
 
The value of 0.1758 (mm^-1^) shown in _exptl_absorpt_coefficient_mu 
is the sample absorption coefficient for neutron wavelength at 1.0 \%A.
;
_shelx_res_checksum              3563
_shelx_hkl_checksum              11754