Synthesis and characterization of zinc di(<i>O</i>-2,2-dimethylpentan-3-yl dithiocarbonates) bearing pyridine or tetramethylethylenediamine coligands and investigation of their thermal conversion mechanisms towards nanocrystalline zinc sulfide.
Vakalopoulou, Efthymia; Buchmaier, Christine; Pein, Andreas; Saf, Robert; Fischer, Roland C.; Torvisco, Ana; Warchomicka, Fernando; Rath, Thomas; Trimmel, Gregor; Dalton transactions (Cambridge, England : 2003) 49 (2020) 14564–14575; doi:10.1039/d0dt03065a

data_7705694
_publ_section_title
;
 Synthesis and characterization of zinc
 di(<i>O</i>-2,2-dimethylpentan-3-yl dithiocarbonates) bearing pyridine or
 tetramethylethylenediamine coligands and investigation of their thermal
 conversion mechanisms towards nanocrystalline zinc sulfide.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14564
_journal_page_last               14575
_journal_paper_doi               10.1039/d0dt03065a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C22 H46 N2 O2 S4 Zn'
_chemical_formula_sum            'C22 H46 N2 O2 S4 Zn'
_chemical_formula_weight         564.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-09-23 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1922(3)
_cell_length_b                   11.5319(3)
_cell_length_c                   22.9826(6)
_cell_measurement_reflns_used    9692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      3.09
_cell_volume                     2966.30(14)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            75890
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.998
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         1.772
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0872 before and 0.0567 after correction.
The Ratio of minimum to maximum transmission is 0.9022.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.270
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3246
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.266
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0349
_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^)+4.9391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3102
_reflns_number_total             3246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03065a2.cif
_cod_data_source_block           wp44b_0m
_cod_depositor_comments
'Adding full bibliography for 7705694--7705695.cif.'
_cod_database_code               7705694
_shelx_shelxl_version_number     2014/7
_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. Shared sites
{C2, C2A}
3. Restrained distances
 C2-C3 \\sim C2-C7 \\sim C2A-C3 \\sim C2A-C7
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C2 \\sim C2A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O1 \\sim O1A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
S2 \\sim S2A \\sim S1 \\sim S1A: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
Uanis(S1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) = Uanis(C1A)
Uanis(C2) = Uanis(C2A)
5. Others
 Sof(H7BC)=Sof(H7BD)=Sof(S1A)=Sof(O1A)=Sof(C1A)=Sof(S2A)=Sof(C2A)=Sof(H2A)=1-
 FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(O1)=Sof(S1)=Sof(S2)=Sof(C1)=Sof(C2)=Sof(H2)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C2A(H2A)
6.b Secondary CH2 refined with riding coordinates:
 C7(H7AA,H7AB), C7(H7BC,H7BD), C10(H10A,H10B)
6.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              1481
_olex2_submission_special_instructions 'No special instructions were received'