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_7248845
_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 Ni, 2(C13 H8 F3 S), 2(C H2 Cl2)'
_chemical_formula_sum            'C32 H20 Cl4 F6 N4 Ni S2'
_chemical_formula_weight         839.168
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2023-10-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-03 deposited with the CCDC.	2024-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                103.512(2)
_cell_angle_beta                 103.720(2)
_cell_angle_gamma                106.570(2)
_cell_formula_units_Z            1
_cell_length_a                   7.5146(3)
_cell_length_b                   10.6915(5)
_cell_length_c                   12.0434(5)
_cell_measurement_reflns_used    8016
_cell_measurement_temperature    105
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.30
_cell_volume                     852.48(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      105
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.9961
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.9971
_diffrn_reflns_Laue_measured_fraction_max 0.9961
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_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            19125
_diffrn_reflns_point_group_measured_fraction_full 0.9971
_diffrn_reflns_point_group_measured_fraction_max 0.9961
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.069
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6675
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0715 before and 0.0351 after correction.
The Ratio of minimum to maximum transmission is 0.8956.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       cube
_exptl_crystal_F_000             423.471
_exptl_crystal_preparation       'slow Diffusion of DCM solutions'
_exptl_crystal_recrystallization_method 'slow Diffusion of DCM solutions'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.3394
_refine_diff_density_min         -0.2839
_refine_diff_density_rms         0.0710
_refine_ls_d_res_high            0.8096
_refine_ls_d_res_low             8.8502
_refine_ls_goodness_of_fit_ref   1.0287
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    19
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0287
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          -0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.5865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0655
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              12
_reflns_limit_k_min              -13
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                2912
_reflns_number_total             3348
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ce00454j2.cif
_cod_data_source_block           P-1_first
_cod_depositor_comments
'Adding full bibliography for 7248845--7248848.cif.'
_cod_database_code               7248845
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C16(H16a,H16b)
1.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C15(H15), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'