Crystal structure of (1,4,7,10,13,16-hexaoxacyclooctadecane-κ6 O)potassium-μ-oxalato-triphenylstannate(IV), the first reported 18-crown-6-stabilized potassium salt of triphenyloxalatostannate
Song, Xueqing; Li, William; Torres, Yolanda; Greaves, Tazena; Acta Crystallographica Section E Crystallographic Communications 80 (2024) –; doi:10.1107/S2056989024007758

data_2023238
_publ_section_title
;
 Crystal structure of (1,4,7,10,13,16-hexaoxacyclooctadecane-\k6
 O)potassium-\m-oxalato-triphenylstannate(IV), the first reported
 18-crown-6-stabilized potassium salt of triphenyloxalatostannate
;
_journal_coeditor_code           NY2007
_journal_issue                   9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024007758
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[K Sn (C6 H5)3 (C2 O4) (C12 H24 O6)]'
_chemical_formula_moiety         'C32 H39 K O10 Sn'
_chemical_formula_sum            'C32 H39 K O10 Sn'
_chemical_formula_weight         741.42
_chemical_name_systematic
(1,4,7,10,13,16-Hexaoxacyclooctadecane-1\k^6^<i>O</i>)(\m-oxalato-1\k^2^<i>O</i>^1^,<i>O</i>^2^:2\k^2^<i>O</i>^1'^,<i>O</i>^2'^)triphenyl-2\k^3^<i>C</i>-potassium(I)tin(IV)
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
FinalCif V138 by Daniel Kratzert, Freiburg 2024,
https://dkratzert.de/finalcif.html
;
_cell_angle_alpha                90
_cell_angle_beta                 97.925(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4060(3)
_cell_length_b                   19.3779(4)
_cell_length_c                   9.4225(3)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.0600
_cell_measurement_theta_min      2.8560
_cell_volume                     1701.02(8)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.62a (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.62a (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.62a (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
Olex2 1.5-beta (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 1.5-beta (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i>  (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'hybrid photon counting'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15412
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.869
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2022)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.032
_exptl_crystal_size_rad          0.021
_refine_diff_density_max         1.280
_refine_diff_density_min         -0.520
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2807 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.08(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7113
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0708P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.1049
_reflns_number_gt                6792
_reflns_number_total             7113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ny2007.cif
_cod_data_source_block           I
_cod_database_code               2023238
_shelx_hkl_checksum              92943
_shelx_res_checksum              50789