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_7061049
_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         'C43 H52 N10 O3 Zn2, 2(Cl O4), C3 H7 N O'
_chemical_formula_sum            'C46 H59 Cl2 N11 O12 Zn2'
_chemical_formula_weight         1159.68
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-20
_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                 99.568(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.008(15)
_cell_length_b                   23.22(2)
_cell_length_c                   16.110(17)
_cell_measurement_reflns_used    8164
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.89
_cell_measurement_theta_min      2.28
_cell_volume                     5167(9)
_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)'5)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.976
_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  0.0827
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47491
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.750
_diffrn_reflns_theta_min         1.715
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.2042 before and 0.0566 after correction.
The Ratio of minimum to maximum transmission is 0.8092.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9647
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_gt           0.0780
_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^)+(0.1558P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4968
_reflns_number_total             9647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03012d2.cif
_cod_data_source_block           Zn2-OH-H2O
_cod_depositor_comments
'Adding full bibliography for 7061049--7061056.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7061049
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.778
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 N1-C13B \\sim N1-C13A
 with sigma of 0.02
 N1-C2A \\sim N1-C2B
 with sigma of 0.02
 C2B-C1 \\sim C2A-C1
 with sigma of 0.02
 C23A-C1 \\sim C23B-C1
 with sigma of 0.02
 N6-C23B \\sim N6-C23A
 with sigma of 0.02
 N6-C24A \\sim N6-C24B
 with sigma of 0.02
 N3-C12B \\sim N3-C11A
 with sigma of 0.02
 C12A-C11A \\sim C12B-C11B
 with sigma of 0.02
 N8-C32A \\sim N8-C32B
 with sigma of 0.02
 C33A-C32A \\sim C33B-C32B
 with sigma of 0.02
 C4-C3A \\sim C4-C3B
 with sigma of 0.02
 N1-C3A \\sim N1-C3B
 with sigma of 0.02
 N6-C34A \\sim N6-C34B
 with sigma of 0.02
 C35-C34A \\sim C35-C34B
 with sigma of 0.02
 N5-C21A \\sim N5-C21B
 with sigma of 0.02
 C22A-C21A \\sim C22B-C21B
 with sigma of 0.02
 C25-C24B \\sim C25-C24A
 with sigma of 0.02
 C14A-C13A \\sim C14B-C13B
 with sigma of 0.02
 Cl2-O9A \\sim Cl2-O9B \\sim Cl2-O8A \\sim Cl2-O8B \\sim Cl2-O11A \\sim
Cl2-O11B \\sim Cl2-O10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24A) = Uanis(C24B)
Uanis(C13A) = Uanis(C13B)
Uanis(C1) = Uanis(C23A) = Uanis(C23B) = Uanis(C2A) = Uanis(C2B)
Uanis(C34A) = Uanis(C34B) = Uanis(C24A) = Uanis(C24B) = Uanis(C3A) = Uanis(C3B)
= Uanis(C13A) = Uanis(C13B)
Uanis(N3) = Uanis(C11A) = Uanis(C11B) = Uanis(C12A) = Uanis(C12B)
Uanis(C32A) = Uanis(C33A)
Uanis(C33B) = Uanis(C32B)
Uanis(N8) = Uanis(C32A) = Uanis(C32B) = Uanis(C33A) = Uanis(C33B)
Uanis(C21A) = Uanis(C21B) = Uanis(C22A) = Uanis(C22B)
Uanis(C14A) = Uanis(C14B)
Uanis(O10) = Uanis(O11A) = Uanis(O11B) = Uanis(O9B) = Uanis(O9A) = Uanis(O8A) =
Uanis(O8B)
4. Others
 Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C11B)=
 Sof(H11C)=Sof(H11D)=Sof(H11E)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(C13B)=
 Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=
 Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=
 Sof(H24C)=Sof(H24D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C33B)=Sof(H33D)=
 Sof(H33E)=Sof(H33F)=Sof(C34B)=Sof(H34C)=Sof(H34D)=Sof(O8B)=Sof(O9B)=Sof(O11B)=
 1-FVAR(1)
 Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C11A)=
 Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13A)=
 Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C22A)=
 Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=
 Sof(H24A)=Sof(H24B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(C33A)=Sof(H33A)=
 Sof(H33B)=Sof(H33C)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(O8A)=Sof(O9A)=Sof(O11A)=
 FVAR(1)
5.a Rotating group:
 O2(H2A,H2B), O3(H3)
5.b Ternary CH refined with riding coordinates:
 C1(H1A), C1(H1B)
5.c Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3A(H3AA,H3AB), C3B(H3BA,H3BB), C11A(H11A,
 H11B), C12B(H12D,H12E), C13A(H13A,H13B), C13B(H13C,H13D), C21A(H21A,H21B),
 C21B(H21C,H21D), C23A(H23A,H23B), C23B(H23C,H23D), C24A(H24A,H24B), C24B(H24C,
 H24D), C32A(H32A,H32B), C32B(H32C,H32D), C34A(H34A,H34B), C34B(H34C,H34D),
 C42(H42A,H42B)
5.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C16(H16), C17(H17), C18(H18), C19(H19),
 C27(H27), C28(H28), C29(H29), C30(H30), C37(H37), C38(H38), C39(H39), C40(H40),
  C46(H46)
5.e Idealised Me refined as rotating group:
 C11B(H11C,H11D,H11E), C12A(H12A,H12B,H12C), C22A(H22A,H22B,H22C), C22B(H22D,
 H22E,H22F), C33A(H33A,H33B,H33C), C33B(H33D,H33E,H33F), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              8613
_olex2_submission_special_instructions 'No special instructions were received'