Formation of extended polyiodides at large cation templates.
Blake, Alexander J.; Castellano, Carlo; Lippolis, Vito; Podda, Enrico; Schröder, Martin; Acta crystallographica. Section C, Structural chemistry 80 (2024) 311–318; doi:10.1107/S2053229624004194

data_2312530
_publ_section_title
;
 Formation of extended polyiodides at large cation templates.
;
_journal_coeditor_code           VP3036
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              311
_journal_page_last               318
_journal_paper_doi               10.1107/S2053229624004194
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Pd2 I2 (C12 H26 N2 S4)] (I)2, 5I2'
_chemical_formula_moiety         'C12 H26 I2 N2 Pd2 S4 2+, 2(I -), 5(I2)'
_chemical_formula_sum            'C12 H26 I14 N2 Pd2 S4'
_chemical_formula_weight         2315.99
_chemical_name_systematic
;
(\m-1,4,10,13-Tetrathia-7,16-diazacyclooctadecane)bis[iodidopalladium(II)]
diiodide penta(diiodine)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.170(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.609(4)
_cell_length_b                   8.198(3)
_cell_length_c                   24.151(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      5
_cell_volume                     4211.1(18)
_computing_cell_refinement
;
STADI4 (Stoe & Cie, 1996)
;
_computing_data_collection
;
STADI4 (Stoe & Cie, 1996)
;
_computing_data_reduction
;
REDU4 (Stoe & Cie, 1996)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 1997)
;
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'STOE STADI4 4-circle'
_diffrn_measurement_method
;
Scan width (omega) = 1.64 - 2.20, scan ratio 2theta:omega = 1.00
 I(Net) and sigma(I) from profile fitting (Clegg, 1981)
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            4584
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         2.663
_diffrn_standards_decay_%        5.0
_diffrn_standards_interval_count 60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.328
_exptl_absorpt_correction_T_max  0.3056
_exptl_absorpt_correction_T_min  0.2217
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(REDU4; Stoe & Cie, 1996)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.653
_exptl_crystal_description       column
_exptl_crystal_F_000             4040
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.349
_refine_diff_density_min         -1.615
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0681P)^2^+91.8532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                3059
_reflns_number_total             3715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vp3036.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 2312530--2312531.cif.'
_cod_database_code               2312530
_shelx_estimated_absorpt_t_min   0.157
_shelx_estimated_absorpt_t_max   0.321
_shelx_hkl_checksum              50346
_shelx_res_checksum              95310