Synthesis and redox reactions of binuclear zinc(ii)–thiolate complexes with elemental sulfur
Naskar, Tilak; Pal, Nabhendu; Majumdar, Amit; New Journal of Chemistry 45 (2021) 22406–22416; doi:10.1039/D1NJ03012D

data_7061056
_publ_section_title
;
 Synthesis and redox reactions of binuclear zinc(ii)--thiolate complexes
 with elemental sulfur
;
_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              22406
_journal_page_last               22416
_journal_paper_doi               10.1039/D1NJ03012D
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C45 H52 N10 O2 S Zn2, 2(Cl O4)'
_chemical_formula_sum            'C45 H52 Cl2 N10 O10 S Zn2'
_chemical_formula_weight         1126.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-10-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0295(5)
_cell_length_b                   23.0096(8)
_cell_length_c                   15.9146(6)
_cell_measurement_reflns_used    18118
_cell_measurement_temperature    148.52
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      2.29
_cell_volume                     5103.8(3)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2016)'
_computing_data_collection       'APEX2 v2017.3-0 (Bruker-Axs,2016)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXD (Sheldrick, 2015)'
_diffrn_ambient_temperature      148.52
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8VENTURE with PHOTON II Detector'
_diffrn_measurement_method       'phi, omega and kappa scan'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            53533
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         2.189
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.150
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1322 before and 0.0656 after correction.
The Ratio of minimum to maximum transmission is 0.7411.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.033
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         9057
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+28.8543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7733
_reflns_number_total             9057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03012d2.cif
_cod_data_source_block           Zn2SCOMe
_cod_depositor_comments
'Adding full bibliography for 7061049--7061056.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7061056
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C20-C15 \\sim C20-C19B \\sim C20-C19A \\sim C19A-C18A \\sim C19B-C18B \\sim
C18A-C17A \\sim C18B-C17B
 \\sim C17A-C16A \\sim C17B-C16B \\sim C16B-C15 \\sim C16A-C15
 with sigma of 0.02
 Cl2-O7 \\sim Cl2-O8A \\sim Cl2-O8B \\sim Cl2-O9B \\sim Cl2-O9A \\sim Cl2-O10B
\\sim Cl2-O10A
 with sigma of 0.02
 C12-C11 \\sim C33A-C32A \\sim C33B-C32B
 with sigma of 0.02
 N7-C26 \\sim N8A-C31 \\sim N8B-C31 \\sim N8B-C25 \\sim N8A-C25
 with sigma of 0.02
 N3-C11 \\sim N8B-C32B \\sim N8A-C33A
 with sigma of 0.02
 Cl1-O3 \\sim Cl1-O6A \\sim Cl1-O6B \\sim Cl1-O5A \\sim Cl1-O5B \\sim Cl1-O4B
\\sim Cl1-O4A
 with sigma of 0.02
 Cl1-O3 \\sim Cl1-O6B \\sim Cl1-O6A \\sim Cl1-O5B \\sim Cl1-O5A \\sim Cl1-O4A
\\sim Cl1-O4B
 with sigma of 0.02
 N6-C24A \\sim N6-C24B
 with sigma of 0.02
 C25-C24B \\sim C25-C24A
 with sigma of 0.02
 C14-C13A \\sim C14-C13B
 with sigma of 0.02
 N1-C13B \\sim N1-C13A
 with sigma of 0.02
 N6-C23B \\sim N6-C23A
 with sigma of 0.02
 C23B-C1 \\sim C23A-C1
 with sigma of 0.02
 C2A-C1 \\sim C2B-C1
 with sigma of 0.02
 N1-C2A \\sim N1-C2B
 with sigma of 0.02
 N1-C3A \\sim N1-C3B
 with sigma of 0.02
 C4-C3A \\sim C4-C3B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O7) = Uanis(O8B) = Uanis(O8A) = Uanis(O9B) = Uanis(O9A) = Uanis(O10A) =
Uanis(O10B)
Uanis(C15) = Uanis(C20) = Uanis(C19B) = Uanis(C19A) = Uanis(C18B) = Uanis(C18A)
= Uanis(C17B) = Uanis(C17A) = Uanis(C16A) = Uanis(C16B)
Uanis(N8A) = Uanis(N8B)
Uanis(C25) = Uanis(C32A) = Uanis(C32B) = Uanis(C33A) = Uanis(C33B)
Uanis(N7) = Uanis(N8A) = Uanis(N8B)
Uanis(O6B) = Uanis(O6A) = Uanis(O5B) = Uanis(O5A) = Uanis(O4A) = Uanis(O4B) =
Uanis(O3)
Uanis(C13A) = Uanis(C13B)
Uanis(C24A) = Uanis(C24B)
Uanis(C23A) = Uanis(C23B)
Uanis(C2A) = Uanis(C2B)
Uanis(C3A) = Uanis(C3B)
4. Others
 Sof(N8B)=Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=
 Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17B)=
 Sof(C18B)=Sof(H18B)=Sof(C19B)=Sof(H19B)=Sof(C23B)=Sof(H23C)=Sof(H23D)=
 Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(C33B)=
 Sof(H33C)=Sof(H33D)=Sof(H33E)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(O8B)=Sof(O9B)=
 Sof(O10B)=1-FVAR(1)
 Sof(N8A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=
 Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=
 Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(O8A)=Sof(O9A)=
 Sof(O10A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1A), C1(H1B)
5.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3A(H3AA,H3AB), C3B(H3BA,H3BB), C11(H11A,
 H11B), C13A(H13A,H13B), C13B(H13C,H13D), C21(H21A,H21B), C23A(H23A,H23B),
 C23B(H23C,H23D), C24A(H24A,H24B), C24B(H24C,H24D), C32B(H32D,H32E), C33A(H33A,
 H33B), C34(H34A,H34B), C42(H42A,H42B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C16A(H16A), C16B(H16B), C17A(H17A),
 C17B(H17B), C18A(H18A), C18B(H18B), C19A(H19A), C19B(H19B), C27(H27), C28(H28),
  C29(H29), C30(H30), C37(H37), C38(H38), C39(H39), C40(H40)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C32A(H32A,H32B,H32C), C33B(H33C,
 H33D,H33E), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              5025
_shelx_fab_checksum              24690
_olex2_submission_special_instructions 'No special instructions were received'