#------------------------------------------------------------------------------
#$Date: 2024-06-13 00:43:35 +0200 (Thu 13 de Jun de 2024) $
#$Revision: 292330 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/88/7248845.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7248845
loop_
_publ_author_name
'Streit, Tim-Niclas'
'Langwald, Jan'
'Gomila, Rosa Maria'
'Frontera, Antonio'
'Malischewski, Moritz'
_publ_section_title
;
 Structural diversity of supramolecular networks formed between
 polycyanometalates and sulfur-based chalcogen bond donors
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D4CE00454J
_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       'φ and ω 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 λ/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/[σ²(Fo²)+(0.0229P)²+0.5865P] where P=(Fo²+2Fc²)/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_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'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ni1 Ni 1.0 0.5 0.5 0.01662(9) Uani 1.000000 2 S T P
S1 S 0.56021(7) 0.61058(5) 0.25356(4) 0.01671(11) Uani 1.000000 1 . . .
Cl1 Cl 0.81812(9) 1.02841(6) 0.65946(5) 0.03682(15) Uani 1.000000 1 . . .
Cl2 Cl 0.93617(9) 0.91552(6) 0.85203(5) 0.03842(15) Uani 1.000000 1 . . .
F3 F 0.23739(19) 0.60661(15) 0.30820(12) 0.0378(3) Uani 1.000000 1 . . .
F2 F 0.4996(2) 0.68656(15) 0.45926(11) 0.0432(4) Uani 1.000000 1 . . .
F1 F 0.3672(2) 0.46974(14) 0.36494(14) 0.0450(4) Uani 1.000000 1 . . .
N1 N 0.6488(3) 0.33539(18) 0.27497(16) 0.0286(4) Uani 1.000000 1 . . .
N2 N 0.9330(3) 0.75566(18) 0.46594(16) 0.0282(4) Uani 1.000000 1 . . .
C4 C 0.5504(3) 0.76725(19) 0.22999(17) 0.0174(4) Uani 1.000000 1 . . .
C5 C 0.3095(3) 0.36768(19) 0.06616(17) 0.0203(4) Uani 1.000000 1 . . .
H5 H 0.3530(3) 0.31563(19) 0.11071(17) 0.0244(5) Uiso 1.000000 1 R . .
C6 C 0.4160(3) 0.74079(19) 0.11668(17) 0.0184(4) Uani 1.000000 1 . . .
C7 C 0.3759(3) 0.50963(19) 0.11184(16) 0.0173(4) Uani 1.000000 1 . . .
C15 C 0.6686(3) 0.8978(2) 0.30964(18) 0.0214(4) Uani 1.000000 1 . . .
H15 H 0.7581(3) 0.9109(2) 0.38338(18) 0.0257(5) Uiso 1.000000 1 R . .
C2 C 0.9631(3) 0.6597(2) 0.48065(17) 0.0202(4) Uani 1.000000 1 . . .
C1 C 0.7836(3) 0.39648(19) 0.36077(18) 0.0203(4) Uani 1.000000 1 . . .
C8 C 0.1841(3) 0.5294(2) -0.06762(17) 0.0207(4) Uani 1.000000 1 . . .
H8 H 0.1421(3) 0.5814(2) -0.11285(17) 0.0249(5) Uiso 1.000000 1 R . .
C9 C 0.1147(3) 0.3863(2) -0.11540(18) 0.0233(4) Uani 1.000000 1 . . .
H9 H 0.0261(3) 0.3431(2) -0.19343(18) 0.0279(5) Uiso 1.000000 1 R . .
C10 C 0.6460(3) 1.0081(2) 0.27309(18) 0.0250(4) Uani 1.000000 1 . . .
H10 H 0.7201(3) 1.0979(2) 0.32389(18) 0.0300(5) Uiso 1.000000 1 R . .
C11 C 0.3993(3) 0.8536(2) 0.08304(18) 0.0227(4) Uani 1.000000 1 . . .
H11 H 0.3121(3) 0.8408(2) 0.00857(18) 0.0273(5) Uiso 1.000000 1 R . .
C3 C 0.4038(3) 0.5925(2) 0.35414(17) 0.0215(4) Uani 1.000000 1 . . .
C12 C 0.1740(3) 0.3063(2) -0.04992(18) 0.0231(4) Uani 1.000000 1 . . .
H12 H 0.1229(3) 0.2107(2) -0.08381(18) 0.0277(5) Uiso 1.000000 1 R . .
C13 C 0.5136(3) 0.9856(2) 0.16139(19) 0.0258(4) Uani 1.000000 1 . . .
H13 H 0.5016(3) 1.0609(2) 0.13870(19) 0.0309(5) Uiso 1.000000 1 R . .
C14 C 0.3171(3) 0.59336(19) 0.04870(16) 0.0174(4) Uani 1.000000 1 . . .
C16 C 0.7903(4) 0.8779(2) 0.70028(19) 0.0335(5) Uani 1.000000 1 . . .
H16a H 0.6534(4) 0.8326(2) 0.69073(19) 0.0402(6) Uiso 1.000000 1 R . .
H16b H 0.8280(4) 0.8151(2) 0.64667(19) 0.0402(6) Uiso 1.000000 1 R . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00313 0.00162 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Cl 0.14908 0.15974 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55740 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
F 0.01756 0.01033 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.27760 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.00612 0.00332 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Ni 0.34081 1.11732 12.83760 7.29200 4.44380 2.38000 3.87850 0.25650 12.17630
66.34210 1.03410 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
S 0.12485 0.12449 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.86690 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Ni1 C2 180.0 . 2_766 ?
C1 Ni1 C2 91.07(8) . 2_766 ?
C1 Ni1 C2 88.93(8) . . ?
C1 Ni1 C2 88.93(8) 2_766 2_766 ?
C1 Ni1 C2 91.07(8) 2_766 . ?
C1 Ni1 C1 180.0 . 2_766 ?
C7 S1 C4 91.97(9) . . ?
C3 S1 C4 99.76(9) . . ?
C3 S1 C7 98.91(9) . . ?
C6 C4 S1 110.82(14) . . ?
C15 C4 S1 124.51(15) . . ?
C15 C4 C6 124.55(18) . . ?
C7 C5 H5 121.67(11) . . ?
C12 C5 H5 121.67(12) . . ?
C12 C5 C7 116.66(18) . . ?
C11 C6 C4 117.42(17) . . ?
C14 C6 C4 113.12(16) . . ?
C14 C6 C11 129.43(18) . . ?
C5 C7 S1 124.48(15) . . ?
C14 C7 S1 111.15(14) . . ?
C14 C7 C5 124.22(17) . . ?
H15 C15 C4 121.88(11) . . ?
C10 C15 C4 116.23(18) . . ?
C10 C15 H15 121.88(12) . . ?
N2 C2 Ni1 177.41(17) . 2_766 ?
N1 C1 Ni1 178.34(18) . 2_766 ?
C9 C8 H8 120.56(12) . . ?
C14 C8 H8 120.56(11) . . ?
C14 C8 C9 118.89(18) . . ?
H9 C9 C8 119.10(12) . . ?
C12 C9 C8 121.81(18) . . ?
C12 C9 H9 119.10(11) . . ?
H10 C10 C15 119.64(12) . . ?
C13 C10 C15 120.72(19) . . ?
C13 C10 H10 119.64(12) . . ?
H11 C11 C6 120.29(11) . . ?
C13 C11 C6 119.42(18) . . ?
C13 C11 H11 120.29(12) . . ?
F3 C3 S1 111.17(13) . . ?
F2 C3 S1 108.76(13) . . ?
F2 C3 F3 109.42(17) . . ?
F1 C3 S1 108.33(13) . . ?
F1 C3 F3 108.93(17) . . ?
F1 C3 F2 110.22(17) . . ?
C9 C12 C5 120.54(18) . . ?
H12 C12 C5 119.73(12) . . ?
H12 C12 C9 119.73(11) . . ?
C11 C13 C10 121.65(19) . . ?
H13 C13 C10 119.18(12) . . ?
H13 C13 C11 119.18(12) . . ?
C7 C14 C6 112.88(16) . . ?
C8 C14 C6 129.19(18) . . ?
C8 C14 C7 117.87(17) . . ?
Cl2 C16 Cl1 111.64(12) . . ?
H16a C16 Cl1 109.29(8) . . ?
H16a C16 Cl2 109.29(8) . . ?
H16b C16 Cl1 109.29(8) . . ?
H16b C16 Cl2 109.29(8) . . ?
H16b C16 H16a 108.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C2 1.864(2) 2_766 ?
Ni1 C2 1.864(2) . ?
Ni1 C1 1.869(2) 2_766 ?
Ni1 C1 1.869(2) . ?
S1 C4 1.7818(19) . ?
S1 C7 1.7780(18) . ?
S1 C3 1.882(2) . ?
Cl1 C16 1.761(2) . ?
Cl2 C16 1.777(2) . ?
F3 C3 1.308(2) . ?
F2 C3 1.301(2) . ?
F1 C3 1.306(2) . ?
N1 C1 1.154(3) . ?
N2 C2 1.154(3) . ?
C4 C6 1.402(3) . ?
C4 C15 1.386(3) . ?
C5 H5 0.9300 . ?
C5 C7 1.379(3) . ?
C5 C12 1.392(3) . ?
C6 C11 1.388(3) . ?
C6 C14 1.465(3) . ?
C7 C14 1.400(3) . ?
C15 H15 0.9300 . ?
C15 C10 1.391(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.391(3) . ?
C8 C14 1.388(3) . ?
C9 H9 0.9300 . ?
C9 C12 1.385(3) . ?
C10 H10 0.9300 . ?
C10 C13 1.391(3) . ?
C11 H11 0.9300 . ?
C11 C13 1.386(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C16 H16a 0.9700 . ?
C16 H16b 0.9700 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C4 C6 C11 -176.96(13) . . . . ?
S1 C4 C6 C14 1.02(15) . . . . ?
S1 C4 C15 C10 177.09(17) . . . . ?
S1 C7 C5 C12 -175.74(16) . . . . ?
S1 C7 C14 C6 -2.13(15) . . . . ?
S1 C7 C14 C8 175.35(13) . . . . ?
C4 C6 C11 C13 -0.1(2) . . . . ?
C4 C6 C14 C7 0.72(18) . . . . ?
C4 C6 C14 C8 -176.40(16) . . . . ?
C4 C15 C10 C13 -1.2(2) . . . . ?
C5 C7 C14 C6 -177.81(19) . . . . ?
C5 C7 C14 C8 -0.3(2) . . . . ?
C5 C12 C9 C8 -1.3(2) . . . . ?
C6 C11 C13 C10 0.3(2) . . . . ?
C6 C14 C8 C9 177.5(2) . . . . ?
C7 C14 C8 C9 0.5(2) . . . . ?
C15 C10 C13 C11 0.4(2) . . . . ?
