Structural diversity of supramolecular networks formed between polycyanometalates and sulfur-based chalcogen bond donors
Streit, Tim-Niclas; Langwald, Jan; Gomila, Rosa M.; Frontera, Antonio; Malischewski, Moritz; CrystEngComm 26 (2024) 3627–3633; doi:10.1039/D4CE00454J

data_7248848
_publ_section_title
;
 Structural diversity of supramolecular networks formed between
 polycyanometalates and sulfur-based chalcogen bond donors
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              3627
_journal_page_last               3633
_journal_paper_doi               10.1039/D4CE00454J
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C8 N8 W, 3(C13 H8 F3 S)'
_chemical_formula_sum            'C47 H24 F9 N8 S3 W'
_chemical_formula_weight         1151.77
_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
_audit_creation_date             2024-04-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-05-03 deposited with the CCDC.	2024-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.077(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.630(5)
_cell_length_b                   14.822(2)
_cell_length_c                   18.028(2)
_cell_measurement_reflns_used    9749
_cell_measurement_temperature    105.00
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      2.26
_cell_volume                     10130(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      105.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            166640
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.375
_diffrn_reflns_theta_min         2.149
_exptl_absorpt_coefficient_mu    2.478
_exptl_absorpt_correction_T_max  0.7406
_exptl_absorpt_correction_T_min  0.6421
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1024 before and 0.0860 after correction.
The Ratio of minimum to maximum transmission is 0.8670.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       plate
_exptl_crystal_F_000             4520
_exptl_crystal_preparation       'Diffusion in DCM'
_exptl_crystal_recrystallization_method 'Diffusion in DCM'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+26.5954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7554
_reflns_number_total             9273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00454j2.cif
_cod_data_source_block           wcn8umef2
_cod_depositor_comments
'Adding full bibliography for 7248845--7248848.cif.'
_cod_database_code               7248848
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.790
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C27(H27), C38(H38), C28(H28), C31(H31), C34(H34), C29(H29),
 C39(H39), C41(H41), C47(H47), C40(H40), C15(H15), C32(H32), C33(H33), C44(H44),
  C46(H46), C13(H13), C14(H14), C22(H22), C19(H19), C12(H12), C45(H45),
 C20(H20), C21(H21)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2380
_shelx_hkl_checksum              73109
_shelx_fab_checksum              34786
_olex2_submission_special_instructions 'No special instructions were received'