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_7248847
_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         'C6 Fe N6, 3(C13 H8 F3 S), C H2 Cl2'
_chemical_formula_sum            'C46 H26 Cl2 F9 Fe N6 S3'
_chemical_formula_weight         1056.66
_chemical_name_systematic        JL-005c
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 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                115.214(2)
_cell_angle_beta                 97.954(2)
_cell_angle_gamma                104.048(2)
_cell_formula_units_Z            1
_cell_length_a                   10.2010(5)
_cell_length_b                   11.0689(11)
_cell_length_c                   11.4836(12)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    105
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.52
_cell_volume                     1094.00(17)
_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
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0531
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            29752
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.035
_diffrn_reflns_theta_min         2.147
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6640
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0620 before and 0.0406 after correction.
The Ratio of minimum to maximum transmission is 0.8909.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             533
_exptl_crystal_preparation       'slow diffusion of soltions in DCM'
_exptl_crystal_recrystallization_method 'Crystallisation Details'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.469(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         8365
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0307P)^2^+0.1823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    0.939
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                7511
_reflns_number_total             8365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00454j2.cif
_cod_data_source_block           fecn6scf3
_cod_depositor_comments
'Adding full bibliography for 7248845--7248848.cif.'
_cod_original_cell_volume        1093.99(17)
_cod_database_code               7248847
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.934
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53072
 0.46928
2.a Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B)
2.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C33(H33), C12(H12), C15(H15), C28(H28), C46(H46), C22(H22),
 C14(H14), C26(H26), C25(H25), C27(H27), C19(H19), C45(H45), C13(H13), C20(H20),
  C30(H30), C34(H34), C21(H21), C40(H40), C44(H44), C41(H41), C29(H29),
 C43(H43), C39(H39)
;
_shelx_res_checksum              14208
_shelx_hkl_checksum              20525
_olex2_submission_special_instructions 'No special instructions were received'