Crystal engineering with short-chained amphiphiles: decasodium octa-<i>n</i>-butanesulfonate di-μ-chlorido-bis[dichloridopalladate(II)] tetrahydrate, a layered inorganic‒organic hybrid material
Thoelen, Felix; Frank, Walter; Acta Crystallographica Section E 75 (2019) 557–561; doi:10.1107/S2056989019004201

data_2242888
_publ_section_title
;
 Crystal engineering with short-chained amphiphiles: decasodium
 octa-<i>n</i>-butanesulfonate di-\m-chlorido-bis[dichloridopalladate(II)]
 tetrahydrate, a layered inorganic--organic hybrid material
;
_journal_coeditor_code           WM5491
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              557
_journal_page_last               561
_journal_paper_doi               10.1107/S2056989019004201
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'Na10 [Pd2 Cl6] (C4 H9 O3 S)8, 4H2 O'
_chemical_formula_moiety
'Cl6 Pd2 2-, 8(C4 H9 O3 S -), 4(H2 O), 10Na +'
_chemical_formula_structural     'Na10 [Pd2 Cl6] (C4 H9 O3 S)8, 4H2 O'
_chemical_formula_sum            'C32 H80 Cl6 Na10 O28 Pd2 S8'
_chemical_formula_weight         1824.84
_chemical_name_systematic
;
Decasodium
octa-<i>n</i>-butanesulfonate di-\m-chlorido-bis[dichloridopalladate(II)]
tetrahydrate
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 94.315(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
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_cell_length_b                   9.9047(2)
_cell_length_c                   22.6734(7)
_cell_measurement_reflns_used    49957
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      59.30
_cell_measurement_theta_min      4.11
_cell_volume                     3561.69(16)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2009)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2009)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2009)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2016)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS_2T'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            48866
_diffrn_reflns_theta_full        27.498
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.132
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>PLATON</i>; Spek, 2009)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_meas      1.712
_exptl_crystal_density_method    'flotation in chloroform/bromoform'
_exptl_crystal_description       'thin platelets'
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.429
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.539
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         8183
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.538
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0215P)^2^+3.8152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                7116
_reflns_number_total             8183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5491sup1.cif
_cod_data_source_block           I
_cod_database_code               2242888
_shelx_estimated_absorpt_t_min   0.650
_shelx_estimated_absorpt_t_max   0.937
_shelx_hkl_checksum              3542
_shelx_res_checksum              88793
_cod_database_fobs_code 2242888