Synthesis and crystal structure of sodium (ethane-1,2-diyl)bis[(3-methoxypropyl)phosphinodithiolate] octahydrate
Nell, Bryan P.; Tyler, David R.; Zakharov, Lev N.; Johnston, Dean H.; Acta Crystallographica Section E Crystallographic Communications 80 (2024) 1138–1141; doi:10.1107/S2056989024009642

data_2023276
_publ_section_title
;
 Synthesis and crystal structure of sodium
 (ethane-1,2-diyl)bis[(3-methoxypropyl)phosphinodithiolate] octahydrate
;
_journal_coeditor_code           EV2010
_journal_issue                   11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1138
_journal_page_last               1141
_journal_paper_doi               10.1107/S2056989024009642
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Na2 (C10 H22 O2 P2 S4) (H2 O)8]'
_chemical_formula_moiety         'C5 H19 Na O5 P S2'
_chemical_formula_sum            'C5 H19 Na O5 P S2'
_chemical_formula_weight         277.28
_chemical_name_systematic
<i>catena</i>-Poly[[triaquasodium]-di-\m-aqua-[triaquasodium]-\m-(ethane-1,2-diyl)bis[(3-methoxypropyl)phosphinodithiolato]]
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                79.608(2)
_cell_angle_beta                 89.207(2)
_cell_angle_gamma                87.0300(10)
_cell_formula_units_Z            2
_cell_length_a                   6.7412(8)
_cell_length_b                   8.2961(8)
_cell_length_c                   11.8621(17)
_cell_measurement_reflns_used    4713
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.50
_cell_volume                     651.63(14)
_computing_cell_refinement
;
SMART (Bruker, 2003)
;
_computing_data_collection
;
SMART (Bruker, 2003)
;
_computing_data_reduction
;
SAINT (Bruker, 2003)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
Olex2 (Dolomanov <i>et al.</i>,  2009) and publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0136
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7596
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.249
_diffrn_reflns_theta_min         2.499
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.837802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             294
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3007
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0357P)^2^+0.2159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                2736
_reflns_number_total             3007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ev2010.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023276.cif.'
_cod_database_code               2023276
_shelx_estimated_absorpt_t_min   0.901
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              65017