The importance of spodium bonds, H-bonds and π-stacking interactions in the solid state structures of four zinc complexes with tetradentate secondary diamine ligands
Middya, Puspendu; Karmakar, Mainak; Gomila, Rosa M.; Drew, Michael G. B.; Frontera, Antonio; Chattopadhyay, Shouvik; New Journal of Chemistry 47 (2023) 9346–9363; doi:10.1039/D2NJ05490F

data_7062406
_publ_section_title
;
 The importance of spodium bonds, H-bonds and \p-stacking interactions in
 the solid state structures of four zinc complexes with tetradentate
 secondary diamine ligands
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9346
_journal_page_last               9363
_journal_paper_doi               10.1039/D2NJ05490F
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C38 H42 Cl4 N4 O8 Zn3, 2(C2 H6 O S)'
_chemical_formula_sum            'C42 H54 Cl4 N4 O10 S2 Zn3'
_chemical_formula_weight         1176.98
_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             2023-03-24
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.03.22 svn.r9e3d6a89 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2023-03-30 deposited with the CCDC.	2023-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                66.030(1)
_cell_angle_beta                 73.559(1)
_cell_angle_gamma                77.067(1)
_cell_formula_units_Z            1
_cell_length_a                   10.2601(2)
_cell_length_b                   11.4484(2)
_cell_length_c                   12.6143(3)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.631
_cell_measurement_theta_min      2.126
_cell_volume                     1288.50(5)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.9940
_diffrn_measured_fraction_theta_max 0.9948
_diffrn_measurement_device_type  'BRUKER D8 QUEST AREA DETECTOR'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.9940
_diffrn_reflns_Laue_measured_fraction_max 0.9948
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            54979
_diffrn_reflns_point_group_measured_fraction_full 0.9940
_diffrn_reflns_point_group_measured_fraction_max 0.9948
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.63
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.729
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.6617
_refine_diff_density_min         -0.5900
_refine_diff_density_rms         0.0582
_refine_ls_d_res_high            0.7188
_refine_ls_d_res_low             9.5804
_refine_ls_extinction_coef       0.0062(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0728
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    50
_refine_ls_number_parameters     323
_refine_ls_number_reflns         7238
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.0702
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.0020
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.6008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0880
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                5996
_reflns_number_total             7272
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj05490f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7062406--7062409.cif.'
_cod_database_code               7062406
_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
 Zn1-O5A \\sim Zn1-O5b
 with sigma of 0.02
 O5A-S1 \\sim O5b-S1a
 with sigma of 0.02
 S1-C20 \\sim S1a-C20a
 with sigma of 0.02
 S1-C21 \\sim S1a-C21a
 with sigma of 0.02
 Zn1-S1 \\sim Zn1-S1a
 with sigma of 0.04
 O5A-C20 \\sim O5b-C20a
 with sigma of 0.04
 O5A-C21 \\sim O5b-C21a
 with sigma of 0.04
 C20-C21 \\sim C20a-C21a
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O5b \\sim S1a \\sim C21a \\sim C20a: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 O5b, S1a, C21a, C20a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O5b)=Sof(C20a)=Sof(S1a)=Sof(C21a)=Sof(H20d)=Sof(H20e)=Sof(H20f)=Sof(H21d)=
 Sof(H21e)=Sof(H21f)=1-FVAR(1)
 Sof(O5A)=Sof(C20)=Sof(S1)=Sof(C21)=Sof(H20a)=Sof(H20b)=Sof(H20c)=Sof(H21a)=
 Sof(H21b)=Sof(H21c)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,H11b)
6.b Me refined with riding coordinates:
 C20a(H20f,H20d,H20e)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2a), C3(H3), C5(H5), C13(H13), C15(H15), C16(H16)
6.d Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C21a(H21d,H21e,
 H21f)
;
_olex2_submission_special_instructions 'No special instructions were received'