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_7061052
_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         'C46 H54 N10 O3 S Zn2, 2(Cl O4)'
_chemical_formula_sum            'C46 H54 Cl2 N10 O11 S Zn2'
_chemical_formula_weight         1156.69
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-16
_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                 95.9880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0208(3)
_cell_length_b                   22.8093(6)
_cell_length_c                   15.7151(4)
_cell_measurement_reflns_used    22642
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.31
_cell_volume                     4998.3(2)
_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      145.35
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51805
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.722
_diffrn_reflns_theta_min         2.211
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1419 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.7841.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.696
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         9461
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0712
_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^)+(0.0896P)^2^+20.4160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.1974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8171
_reflns_number_total             9461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03012d2.cif
_cod_data_source_block           Zn2mercaptopropionic
_cod_depositor_comments
'Adding full bibliography for 7061049--7061056.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7061052
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.765
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All S(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C46B-C45 \\sim C46A-C45
 with sigma of 0.02
 N8-C32A \\sim N8-C32B
 with sigma of 0.02
 N3-C11 \\sim N8-C32A \\sim N8-C32B
 with sigma of 0.02
 C12-C11 \\sim C32A-C33A \\sim C32B-C33B
 with sigma of 0.02
 Cl2-O10A \\sim Cl2-O10B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C45) = Uanis(C46A) = Uanis(C46B)
Uanis(O7B) = Uanis(O7A) = Uanis(O6A) = Uanis(O6B)
Uanis(C33A) = Uanis(C32A)
Uanis(C25) = Uanis(C33B) = Uanis(C32B)
Uanis(O10A) = Uanis(O10B)
4. Others
 Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=
 Sof(H45C)=Sof(H45D)=Sof(C46B)=Sof(H46C)=Sof(H46D)=Sof(O6B)=Sof(O7B)=Sof(O10B)=
 Sof(H1B)=1-FVAR(1)
 Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(H45A)=Sof(H45B)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(O6A)=Sof(O7A)=Sof(O10A)=
 Sof(H1A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C13(H13A,H13B), C21(H21A,H21B),
 C23(H23A,H23B), C24(H24A,H24B), C32A(H32A,H32B), C32B(H32C,H32D), C34(H34A,
 H34B), C42(H42A,H42B), C45(H45A,H45B), C45(H45C,H45D), C46A(H46A,H46B),
 C46B(H46C,H46D)
5.c 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)
5.d Tetrahedral OH refined with riding coordinates:
 S1(H1A), S1(H1B)
5.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C33A(H33A,H33B,H33C), C33B(H33D,
 H33E,H33F), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              56417
_olex2_submission_special_instructions 'No special instructions were received'