High-speed electrodeposition of copper-tin-zinc stacks from liquid metal salts for Cu2ZnSnSe4 solar cells.
Steichen, Marc; Malaquias, João C; Arasimowicz, Monika; Djemour, Rabie; Brooks, Neil R.; Van Meervelt, Luc; Fransaer, Jan; Binnemans, Koen; Dale, Phillip J.; Chemical communications (Cambridge, England) 53 (2017) 913–916; doi:10.1039/c6cc09225j

data_7119227
_publ_section_title
;
 High-speed electrodeposition of copper-tin-zinc stacks from liquid metal
 salts for Cu2ZnSnSe4 solar cells.
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              913
_journal_page_last               916
_journal_paper_doi               10.1039/c6cc09225j
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C8 H20 O4 Sn, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C12 H20 F12 N2 O12 S4 Sn'
_chemical_formula_weight         859.23
_chemical_melting_point          332
_chemical_name_systematic
'tin 1-methoxy-2-(2-methoxyethoxy)ethane ethanolbis(trifluoromethylsulfonyl)imide'
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-06-24
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5059)
;
_audit_update_record
;
2016-02-08 deposited with the CCDC.
2016-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                85.032(3)
_cell_angle_beta                 80.364(3)
_cell_angle_gamma                67.851(4)
_cell_formula_units_Z            2
_cell_length_a                   9.1134(3)
_cell_length_b                   9.5041(4)
_cell_length_c                   18.0048(7)
_cell_measurement_reflns_used    5839
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6140
_cell_measurement_theta_min      3.0950
_cell_volume                     1423.55(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_details
;
  1 omega  -45.00   53.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513   77.0000  -60.0000 98

  2 omega  -24.00   37.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513   57.0000   90.0000 61

  3 omega  -86.00    0.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513  -57.0000 -180.0000 86

  4 omega  -10.00   79.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0263   77.0000  150.0000 89

  5 omega    2.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0263   57.0000   60.0000 68
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0064777000
_diffrn_orient_matrix_UB_12      0.0225295000
_diffrn_orient_matrix_UB_13      -0.0382842000
_diffrn_orient_matrix_UB_21      0.0674052000
_diffrn_orient_matrix_UB_22      -0.0660016000
_diffrn_orient_matrix_UB_23      -0.0114670000
_diffrn_orient_matrix_UB_31      -0.0512566000
_diffrn_orient_matrix_UB_32      -0.0403522000
_diffrn_orient_matrix_UB_33      -0.0005751000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11850
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         2.84
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_recrystallization_method
'slow crystallization at RT on vacuum line'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.068
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         6476
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.9557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                6068
_reflns_number_total             6476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc09225j2.cif
_cod_data_source_block           nrb129
_cod_depositor_comments          'Adding full bibliography for 7119227.cif.'
_cod_database_code               7119227
_chemical_oxdiff_formula         'Sn C4 F12 N2 S4 O8 C12 H28 O6'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C41-F42 \\sim C41-F43 \\sim C41-F44 \\sim C52-F53 \\sim C52-F54 \\sim C52-F55
 with sigma of 0.01
 F42-F43 \\sim F42-F44 \\sim F43-F44 \\sim F53-F54 \\sim F53-F55 \\sim F54-F55
 with sigma of 0.02
 C61-F62 \\sim C61-F63 \\sim C61-F64 \\sim C72-F73 \\sim C72-F74 \\sim C72-F75
 with sigma of 0.01
 F62-F63 \\sim F62-F64 \\sim F63-F64 \\sim F73-F74 \\sim F73-F75 \\sim F74-F75
 with sigma of 0.02
 C2-C3 \\sim C2'-C3'
 with sigma of 0.01
 O1-C2 \\sim O1-C2'
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C41 \\sim F42 \\sim F43 \\sim F44 \\sim S45 \\sim O46 \\sim O47 \\sim N48 \\sim
S49 \\sim O50 \\sim O51 \\sim C52 \\sim F53 \\sim F54 \\sim F55 \\sim C61 \\sim
F62 \\sim F63 \\sim F64 \\sim S65 \\sim O66 \\sim O67 \\sim N68 \\sim S69 \\sim
O70 \\sim O71 \\sim C72 \\sim F73 \\sim F74 \\sim F75: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C2) = Uanis(C2')
Uanis(C3) = Uanis(C3')
4. Others
 Sof(C2')=Sof(H2'A)=Sof(H2'B)=Sof(C3')=Sof(H3'A)=Sof(H3'B)=Sof(H3'C)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
 Fixed Sof: C41(0.5) F42(0.5) F43(0.5) F44(0.5) S45(0.5) O46(0.5) O47(0.5)
 N48(0.5) S49(0.5) O50(0.5) O51(0.5) C52(0.5) F53(0.5) F54(0.5) F55(0.5)
 C61(0.5) F62(0.5) F63(0.5) F64(0.5) S65(0.5) O66(0.5) O67(0.5) N68(0.5)
 S69(0.5) O70(0.5) O71(0.5) C72(0.5) F73(0.5) F74(0.5) F75(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C2'(H2'A,
 H2'B)
5.b Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C12(H12A,H12B,H12C)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3'(H3'A,H3'B,H3'C)
;
_olex2_date_sample_data_collection 2013-03-08
_olex2_submission_special_instructions 'No special instructions were received'