A New Bis(thioether)-Dipyrrin N2S2 Ligand and Its Coordination Behaviors to Nickel, Copper and Zinc
Wu, Tengdie; Wang, Shen; Lv, Yongxin; Fu, Tianyue; Jiang, Jinhai; Lu, Xin; Yu, Zhi-Peng; zhang, jie; Wang, Lianke; Zhou, Hong-Ping; Dalton Transactions  (2022) –; doi:10.1039/D2DT01282K

data_7710336
_publ_section_title
;
 A New Bis(thioether)-Dipyrrin N2S2 Ligand and Its Coordination Behaviors
 to Nickel, Copper and Zinc
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01282K
_journal_year                    2022
_chemical_formula_moiety         'C66 H50 Cl2 F12 N4 Ni2 S4'
_chemical_formula_sum            'C66 H50 Cl2 F12 N4 Ni2 S4'
_chemical_formula_weight         1443.66
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-06 deposited with the CCDC.	2022-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                69.290(2)
_cell_angle_beta                 70.236(2)
_cell_angle_gamma                85.129(3)
_cell_formula_units_Z            1
_cell_length_a                   10.3025(17)
_cell_length_b                   12.284(2)
_cell_length_c                   14.517(2)
_cell_measurement_reflns_used    1588
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.323
_cell_measurement_theta_min      2.494
_cell_volume                     1616.0(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0934
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11770
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.589
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0573 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.8735.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         5658
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0565P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3304
_reflns_number_total             5658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01282k2.cif
_cod_data_source_block           1_CCDC1
_cod_original_cell_volume        1616.1(5)
_cod_database_code               7710336
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.859
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C20-C16 = C20A-C16
 1.54 with sigma of 0.01
 F2A-C20A = C20A-F1A
 1.38 with sigma of 0.02
 F1A-C20A = C20A-F3A
 1.38 with sigma of 0.02
 F1-C20 = C20-F3
 1.38 with sigma of 0.02
 F3-C20 = C20-F2
 1.38 with sigma of 0.02
 F3A-C20A = C20A-F2A
 1.38 with sigma of 0.02
 F2-C20 = C20-F1
 1.38 with sigma of 0.02
 F1-F3
 2.384 with sigma of 0.04
 F2-F1
 2.384 with sigma of 0.04
 F3A-F2A
 2.384 with sigma of 0.04
 F3-F2
 2.384 with sigma of 0.04
 F2A-F1A
 2.384 with sigma of 0.04
 F1A-F3A
 2.384 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C15 \\sim C14 \\sim C19 \\sim C18 \\sim C17 \\sim C16: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
F1 \\sim F2 \\sim F3 \\sim C20 \\sim F1A \\sim F2A \\sim F3A \\sim C20A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 F4A, F6A, F5A, C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 F4, C21, F6, F5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 F2, F3, F1, C20, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C16, F2A, C20A, F3A, F1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(C20A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C20)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C10(H10), C11(H11), C15(H15), C17(H17), C19(H19),
 C23(H23), C24(H24), C27(H27), C30(H30), C31(H31)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C012(H01A,H01B,H01C), C29(H29A,H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'