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_7248846
_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         'C4 N4 Zn, 2(C13 H8 F3 S), C H2 Cl2, H2 O'
_chemical_formula_sum            'C31 H20 Cl2 F6 N4 O S2 Zn'
_chemical_formula_weight         778.90
_chemical_name_systematic        'TNS ZnCN4'
_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   mixed
_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                105.866(2)
_cell_angle_beta                 107.532(2)
_cell_angle_gamma                94.354(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2339(4)
_cell_length_b                   13.5275(7)
_cell_length_c                   14.9019(8)
_cell_measurement_reflns_used    6449
_cell_measurement_temperature    105.0
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.51
_cell_volume                     1681.72(15)
_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 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0678
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23898
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.402
_diffrn_reflns_theta_min         1.818
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6417
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0928 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.8611.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_preparation       'Diffusion of DCM'
_exptl_crystal_recrystallization_method 'Diffusion of DCM'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0287P)^2^+1.1597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4575
_reflns_number_total             6162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00454j2.cif
_cod_data_source_block           p-1_full
_cod_depositor_comments
'Adding full bibliography for 7248845--7248848.cif.'
_cod_database_code               7248846
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.900
_olex2_refinement_description
;
1.a Free rotating group:
 O2(H2A,H2B)
1.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
1.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C18(H18), C19(H19), C12(H12), C23(H23), C13(H13), C24(H24),
 C26(H26), C27(H27), C14(H14), C28(H28), C15(H15), C16(H16), C30(H30), C29(H29),
  C17(H17)
;
_shelx_res_checksum              87171
_shelx_hkl_checksum              7236
_olex2_submission_special_instructions 'No special instructions were received'