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_7061050
_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 H54 N10 O S Zn2, 2(B F4)'
_chemical_formula_sum            'C45 H54 B2 F8 N10 O S Zn2'
_chemical_formula_weight         1087.40
_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             2021-10-22
_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                 98.363(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2217(7)
_cell_length_b                   22.1402(12)
_cell_length_c                   15.7926(8)
_cell_measurement_reflns_used    15789
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.25
_cell_volume                     4919.8(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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0746
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46038
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.072
_diffrn_reflns_theta_max         25.072
_diffrn_reflns_theta_min         2.255
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1209 before and 0.0768 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    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.958
_refine_diff_density_min         -1.327
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         8713
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0746
_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^)+(0.1060P)^2^+22.1206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7295
_reflns_number_total             8713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03012d2.cif
_cod_data_source_block           Zn2SEt
_cod_depositor_comments
'Adding full bibliography for 7061049--7061056.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7061050
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.795
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F2-B1 \\sim F3-B1 \\sim F1A-B1 \\sim F1B-B1 \\sim F4A-B1 \\sim F4B-B1
 with sigma of 0.02
 F6B-B2B \\sim F6A-B2A \\sim F8A-B2A \\sim F8B-B2B \\sim F7B-B2B \\sim F7A-B2A
\\sim F5A-B2A \\sim F5B-B2B
 with sigma of 0.02
 C41-C36 \\sim C37-C36 \\sim C38A-C37 \\sim C38B-C37 \\sim C39A-C38A \\sim
C39B-C38B \\sim C40A-C39A ~
 C40B-C39B \\sim C41-C40B \\sim C41-C40A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12B) = Uanis(C12A)
Uanis(F1A) = Uanis(F1B)
Uanis(F4A) = Uanis(F4B)
Uanis(F8B) = Uanis(F8A) = Uanis(F7B) = Uanis(F7A)
Uanis(B2A) = Uanis(B2B) = Uanis(F6B) = Uanis(F6A)
Uanis(F5B) = Uanis(F5A)
Uanis(C36) = Uanis(C41) = Uanis(C40A) = Uanis(C40B) = Uanis(C39A) = Uanis(C39B)
= Uanis(C38B) = Uanis(C38A) = Uanis(C37)
Uanis(F2) = Uanis(F1A) = Uanis(F1B) = Uanis(F4A) = Uanis(F4B)
4. Others
 Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(H32C)=
 Sof(H32D)=Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(H37A)=Sof(C38B)=
 Sof(H38B)=Sof(C39B)=Sof(H39B)=Sof(C40B)=Sof(H40B)=Sof(F1B)=Sof(F4B)=Sof(F5B)=
 Sof(F6B)=Sof(F7B)=Sof(F8B)=Sof(B2B)=1-FVAR(1)
 Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(H32A)=
 Sof(H32B)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(H37)=Sof(C38A)=Sof(H38A)=
 Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=Sof(F1A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=
 Sof(F7A)=Sof(F8A)=Sof(B2A)=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), C11(H11C,H11D), C13(H13A,H13B),
 C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C32(H32A,H32B), C32(H32C,H32D),
  C34(H34A,H34B), C42(H42A,H42B), C44(H44A,H44B)
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), C37(H37A), C38A(H38A),
 C38B(H38B), C39A(H39A), C39B(H39B), C40A(H40A), C40B(H40B)
5.d Idealised Me refined as rotating group:
 C12A(H12A,H12B,H12C), C12B(H12D,H12E,H12F), C22(H22A,H22B,H22C), C33A(H33A,
 H33B,H33C), C33B(H33D,H33E,H33F), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              70961
_olex2_submission_special_instructions 'No special instructions were received'