Synthesis and anion binding properties of (thio)urea functionalized Ni(II)-salen complexes.
Payong, Jae Elise L.; Léonard, Nadia G; Anderson-Sanchez, Lauren M; Ziller, Joseph W.; Yang, Jenny Y.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 934–941; doi:10.1039/d4dt02683g

data_7717355
_publ_section_title
;
 Synthesis and anion binding properties of (thio)urea functionalized
 Ni(II)-salen complexes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              934
_journal_page_last               941
_journal_paper_doi               10.1039/d4dt02683g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'1(C32 H30 N6 Ni O2 S2), C2 H6 O S, 0.6[C2H6SO]'
_chemical_formula_sum            'C35.2 H39.6 N6 Ni O3.6 S3.6'
_chemical_formula_weight         778.45
_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   geom
_audit_creation_date             2024-08-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-08-24 deposited with the CCDC.	2024-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                79.477(2)
_cell_angle_beta                 86.598(2)
_cell_angle_gamma                88.997(2)
_cell_formula_units_Z            4
_cell_length_a                   13.4469(4)
_cell_length_b                   14.7117(5)
_cell_length_c                   18.4767(7)
_cell_measurement_reflns_used    9420
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      72.16
_cell_measurement_theta_min      3.55
_cell_volume                     3587.3(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      93.15
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker X8 Prospector APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            94171
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.674
_diffrn_reflns_theta_min         2.436
_diffrn_source_current           0.65
_diffrn_source_power             0.029094000000000002
_diffrn_source_voltage           44.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.119
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1153 before and 0.0796 after correction.
The Ratio of minimum to maximum transmission is 0.6972.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       trapezoidal
_exptl_crystal_F_000             1629
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMSO/methyl tert-butyl ether'
_exptl_crystal_size_max          0.431
_exptl_crystal_size_mid          0.323
_exptl_crystal_size_min          0.088
_refine_diff_density_max         1.148
_refine_diff_density_min         -2.005
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         13642
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0742
_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^)+(0.0810P)^2^+14.9981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.2016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10805
_reflns_number_total             13642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02683g2.cif
_cod_data_source_block           jyy315
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7717351--7717355.cif.
;
_cod_original_formula_sum        'C35.20 H39.60 N6 Ni O3.60 S3.60'
_cod_database_code               7717355
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.771
_shelx_estimated_absorpt_t_min   0.347
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4A-C19 \\sim N4B-C19
 with sigma of 0.02
 N4A-C20A \\sim N4B-C20B
 with sigma of 0.02
 C20A-C21A \\sim C20B-C21B
 with sigma of 0.02
 C20A-C25A \\sim C20B-C25B
 with sigma of 0.02
 C22A-C21A \\sim C22B-C21B
 with sigma of 0.02
 C22A-C23A \\sim C22B-C23B
 with sigma of 0.02
 C25A-C24A \\sim C25B-C24B
 with sigma of 0.02
 C24A-C23A \\sim C24B-C23B
 with sigma of 0.02
 N4A-C21A \\sim N4B-C21B
 with sigma of 0.04
 N4A-C25A \\sim N4B-C25B
 with sigma of 0.04
 C19-C20A \\sim C19-C20B
 with sigma of 0.04
 C20A-C22A \\sim C20B-C22B
 with sigma of 0.04
 C20A-C24A \\sim C20B-C24B
 with sigma of 0.04
 C22A-C24A \\sim C22B-C24B
 with sigma of 0.04
 C21A-C25A \\sim C21B-C25B
 with sigma of 0.04
 C21A-C23A \\sim C21B-C23B
 with sigma of 0.04
 C25A-C23A \\sim C25B-C23B
 with sigma of 0.04
 N12B-C62A \\sim N12B-C62B
 with sigma of 0.02
 C62A-C63A \\sim C62B-C63B
 with sigma of 0.02
 C62A-C67B \\sim C62B-C67A
 with sigma of 0.02
 C63A-C64A \\sim C63B-C64B
 with sigma of 0.02
 C64A-C65B \\sim C64B-C65A
 with sigma of 0.02
 C65B-C66B \\sim C65A-C66A
 with sigma of 0.02
 C67B-C66B \\sim C67A-C66A
 with sigma of 0.02
 N12B-C63A \\sim N12B-C63B
 with sigma of 0.04
 N12B-C67B \\sim N12B-C67A
 with sigma of 0.04
 C62A-C64A \\sim C62B-C64B
 with sigma of 0.04
 C62A-C66B \\sim C62B-C66A
 with sigma of 0.04
 C63A-C65B \\sim C63B-C65A
 with sigma of 0.04
 C63A-C67B \\sim C63B-C67A
 with sigma of 0.04
 C64A-C66B \\sim C64B-C66A
 with sigma of 0.04
 C65B-C67B \\sim C65A-C67A
 with sigma of 0.04
 N12B-C61 \\sim N12A-C61
 with sigma of 0.02
 N12B-C62A \\sim N12A-C62A
 with sigma of 0.02
 N12B-C62B \\sim N12A-C62B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N12A \\sim C62A \\sim C63A \\sim C64A \\sim C65A \\sim C66A \\sim C67A: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(N12A) \\sim Ueq, Uanis(C62A) \\sim Ueq, Uanis(C67A) \\sim Ueq,
Uanis(C66A) \\sim Ueq, Uanis(C65A) \\sim Ueq, Uanis(C64A) \\sim Ueq,
Uanis(C63A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C23B) = Uanis(C22B) = Uanis(C24B) = Uanis(C21B) = Uanis(C25B) =
Uanis(N4B) = Uanis(C20B)
Uanis(N4A) = Uanis(C24A) = Uanis(C20A) = Uanis(C25A) = Uanis(C22A) =
Uanis(C23A) = Uanis(C21A)
Uanis(N12B) = Uanis(C62B) = Uanis(C63B) = Uanis(C64B) = Uanis(C65B) =
Uanis(C66B) = Uanis(C67B)
Uanis(C34) = Uanis(S3) = Uanis(O3) = Uanis(C35)
4. Others
 Fixed Sof: N12B(0.35) H12D(0.35) N4A(0.5) H4A(0.5) C62A(0.65) C63A(0.65)
 H63A(0.65) C64A(0.65) H64A(0.65) C65B(0.35) H65B(0.35) C20A(0.5) C67B(0.35)
 H67B(0.35) C22A(0.5) H22A(0.5) C66B(0.35) H66B(0.35) C21A(0.5) H21A(0.5)
 C25A(0.5) H25A(0.5) C24A(0.5) H24A(0.5) C23A(0.5) H23A(0.5) C23B(0.5)
 H23B(0.5) C24B(0.5) H24B(0.5) C25B(0.5) H25B(0.5) C20B(0.5) C21B(0.5)
 H21B(0.5) C22B(0.5) H22B(0.5) N4B(0.5) H4B(0.5) C64B(0.35) H64B(0.35)
 C63B(0.35) H63B(0.35) C62B(0.35) C65A(0.65) H65A(0.65) C66A(0.65) H66A(0.65)
 C67A(0.65) H67A(0.65) N12A(0.65) H12E(0.65)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C44(H44A,H44B), C9(H9A,H9B), C20(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), N11(H11), N9(H9), N6(H6), N12B(H12D), N10(H10), C4(H4),
 C5(H5A), C3(H3A), C51(H51), C49(H49), C14(H14), C40(H40), C38(H38), N4A(H4A),
 C16(H16), C50(H50), C39(H39), C15(H15), C63A(H63A), C59(H59), C56(H56),
 C60(H60), C29(H29), C58(H58), C57(H57), C33(H33), C32(H32), C64A(H64A),
 C65B(H65B), C30(H30), C31(H31), C67B(H67B), C22A(H22A), C66B(H66B), C21A(H21A),
  C25A(H25A), C24A(H24A), C23A(H23A), C23B(H23B), C24B(H24B), C25B(H25B),
 C21B(H21B), C22B(H22B), N4B(H4B), C64B(H64B), C63B(H63B), C65A(H65A),
 C66A(H66A), C67A(H67A), N12A(H12E)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C43(H43A,H43B,H43C), C47(H47A,H47B,
 H47C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 102 electrons were 
found in a volume of 357\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.6[C2H6SO] per Asymmetric Unit 
which account for 101 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93108
_shelx_fab_checksum              62740
_olex2_submission_special_instructions 'No special instructions were received'