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_7061054
_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         'C50 H54 N10 O3 S Zn2, 2(B F4), 2(C3 H7 N O)'
_chemical_formula_sum            'C56 H68 B2 F8 N12 O5 S Zn2'
_chemical_formula_weight         1325.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-05
_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                 111.4350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.8019(6)
_cell_length_b                   15.1522(3)
_cell_length_c                   29.4177(6)
_cell_measurement_reflns_used    25488
_cell_measurement_temperature    146(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.47
_cell_volume                     11950.3(4)
_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      146(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0328
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            60678
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.066
_diffrn_reflns_theta_max         25.066
_diffrn_reflns_theta_min         2.475
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1092 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.8476.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5488
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.717
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         10512
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0811
_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^)+(0.1054P)^2^+104.2883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2110
_refine_ls_wR_factor_ref         0.2181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9187
_reflns_number_total             10512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03012d2.cif
_cod_data_source_block           Zn2mercaptobenzoic
_cod_depositor_comments
'Adding full bibliography for 7061049--7061056.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7061054
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.809
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All S(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N5A-C21A \\sim N5B-C21B
 with sigma of 0.02
 C22A-C21A \\sim C22B-C21B
 with sigma of 0.02
 N12-C56B \\sim N12-C56A
 with sigma of 0.02
 N12-C54A \\sim N12-C54B \\sim N12-C55B \\sim N12-C55A
 with sigma of 0.02
 N11-C51 \\sim N11-C52A \\sim N11-C52B
 with sigma of 0.02
 F6A-B2A \\sim F5A-B2A \\sim F8A-B2A \\sim F7A-B2A \\sim F8B-B2B \\sim F6B-B2B
\\sim F5B-B2B
 with sigma of 0.02
 C20-C15 \\sim C16-C15 \\sim C17-C16 \\sim C18-C17 \\sim C19B-C18 \\sim
C19A-C18 \\sim C20-C19B \\sim C20-
 C19A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C21B) = Uanis(C21A)
Uanis(C22B) = Uanis(C22A)
Uanis(C52B) = Uanis(C52A)
Uanis(B2B) = Uanis(B2A)
Uanis(F5A) = Uanis(F5B) = Uanis(F6A) = Uanis(F6B) = Uanis(F7A) = Uanis(F7B) =
Uanis(F8A) = Uanis(F8B)
Uanis(C51) = Uanis(C52B) = Uanis(C52A)
Uanis(C56A) = Uanis(C56B)
Uanis(C54A) = Uanis(C54B)
Uanis(C55A) = Uanis(C55B)
Uanis(F2) = Uanis(F4B) = Uanis(F4A)
Uanis(N4) = Uanis(N5A) = Uanis(N5B)
4. Others
 Sof(N5B)=Sof(H18A)=Sof(C19B)=Sof(H19B)=Sof(C21B)=Sof(H21C)=Sof(H21D)=
 Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(F7B)=
 Sof(F8B)=Sof(B2B)=Sof(C52B)=Sof(H52D)=Sof(H52E)=Sof(H52F)=Sof(C54B)=Sof(H54D)=
 Sof(H54E)=Sof(H54F)=Sof(C55B)=Sof(H55D)=Sof(H55E)=Sof(H55F)=Sof(C56B)=
 Sof(H56B)=1-FVAR(1)
 Sof(N5A)=Sof(H18)=Sof(C19A)=Sof(H19A)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C22A)=
 Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=
 Sof(B2A)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C54A)=Sof(H54A)=Sof(H54B)=
 Sof(H54C)=Sof(C55A)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C56A)=Sof(H56A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1A)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C13(H13A,H13B), C21A(H21A,H21B),
 C21B(H21C,H21D), C23(H23A,H23B), C24(H24A,H24B), C32(H32A,H32B), C34(H34A,
 H34B), C42(H42A,H42B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C16(H16), C17(H17), C18(H18), C18(H18A),
 C19A(H19A), C19B(H19B), C27(H27), C28(H28), C29(H29), C30(H30), C37(H37),
 C38(H38), C39(H39), C40(H40), C46(H46), C47(H47), C49(H49), C50(H50), C53(H53),
  C56A(H56A), C56B(H56B)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F), C33(H33A,
 H33B,H33C), C43(H43A,H43B,H43C), C51(H51A,H51B,H51C), C52A(H52A,H52B,H52C),
 C52B(H52D,H52E,H52F), C54A(H54A,H54B,H54C), C54B(H54D,H54E,H54F), C55A(H55A,
 H55B,H55C), C55B(H55D,H55E,H55F)
5.e Idealised tetrahedral OH refined as rotating group:
 S1(H1)
;
_shelx_res_checksum              61316
_olex2_submission_special_instructions 'No special instructions were received'