Homoleptic trimethylsilylchalcogenolato zincates [Zn(ESiMe<sub>3</sub>)<sub>3</sub>]<sup>-</sup> and stannanides [Sn(ESiMe<sub>3</sub>)<sub>3</sub>]<sup>-</sup> (E = S, Se): precursors in solution-based low-temperature binary metal chalcogenide and Cu<sub>2</sub>ZnSnS<sub>4</sub> (CZTS) synthesis.
Guschlbauer, Jannick; Vollgraff, Tobias; Sundermeyer, Jörg; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2517–2526; doi:10.1039/c9dt04144c

data_7703406
_publ_section_title
;
 Homoleptic trimethylsilylchalcogenolato zincates
 [Zn(ESiMe<sub>3</sub>)<sub>3</sub>]<sup>-</sup> and stannanides
 [Sn(ESiMe<sub>3</sub>)<sub>3</sub>]<sup>-</sup> (E = S, Se): precursors
 in solution-based low-temperature binary metal chalcogenide and
 Cu<sub>2</sub>ZnSnS<sub>4</sub> (CZTS) synthesis.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2517
_journal_page_last               2526
_journal_paper_doi               10.1039/c9dt04144c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C18 H54 Se6 Si6 Zn2, 2(C24 H20 P)'
_chemical_formula_sum            'C66 H94 P2 Se6 Si6 Zn2'
_chemical_formula_weight         1722.39
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-07-15 deposited with the CCDC.	2020-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                104.645(14)
_cell_angle_beta                 108.529(13)
_cell_angle_gamma                105.841(14)
_cell_formula_units_Z            1
_cell_length_a                   12.360(6)
_cell_length_b                   12.641(6)
_cell_length_c                   14.290(7)
_cell_measurement_reflns_used    9298
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.6700
_cell_measurement_theta_min      2.5375
_cell_volume                     1890.2(16)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service v3.0.26'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics
'DIAMOND 4 (H. Putz, K. Brandenburg, Crystal Impact GbR, Kreuzherrenstr. 102, 53227 Bonn, Germany)'
_computing_publication_material
'WinGX 2014.1 (L.J. Farrugia, J. Appl. Cryst. 2012, 45, 849-854)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'D8 Quest (Bruker AXS Inc.)'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            53377
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.748
_diffrn_reflns_theta_min         2.540
_diffrn_source                   'I\mS Microfocus Source'
_exptl_absorpt_coefficient_mu    3.697
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.205
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7214
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0222P)^2^+2.0610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5943
_reflns_number_total             7214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04144c2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7703404--7703406.cif.'
_cod_original_cell_volume        1890.2(17)
_cod_database_code               7703406
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.468
_shelx_estimated_absorpt_t_max   0.518
_exptl_absorpt_special_details
'SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10.'
_shelx_res_checksum              83754