Additive-free spin coating of tin oxide thin films: synthesis, characterization and evaluation of tin β-ketoiminates as a new precursor class for solution deposition processes.
Huster, Niklas; Zanders, David; Karle, Sarah; Rogalla, Detlef; Devi, Anjana; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10755–10764; doi:10.1039/d0dt01463j

data_7704579
_publ_section_title
;
 Additive-free spin coating of tin oxide thin films: synthesis,
 characterization and evaluation of tin \b-ketoiminates as a new precursor
 class for solution deposition processes.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10755
_journal_page_last               10764
_journal_paper_doi               10.1039/d0dt01463j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C18 H32 N2 O4 Sn'
_chemical_formula_sum            'C18 H32 N2 O4 Sn'
_chemical_formula_weight         459.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-17 deposited with the CCDC.	2020-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1801(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.28458(9)
_cell_length_b                   15.15852(17)
_cell_length_c                   16.5128(2)
_cell_measurement_reflns_used    8332
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.9140
_cell_measurement_theta_min      3.9670
_cell_volume                     2068.19(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -102.00 -23.00   0.50    0.05    --  -47.45 -80.00-174.00  158
  2  \w     12.00  47.00   0.50    0.05    --   47.45 -80.00-174.00   70
  3  \w     57.00  83.00   0.50    0.07    --  106.49 -80.00-174.00   52
  4  \w     51.00 101.00   0.50    0.07    --  106.49 -94.00 -90.00  100
  5  \w     36.00  69.00   0.50    0.07    --  106.49 -61.00-150.00   66
  6  \w     34.00  74.00   0.50    0.07    --  106.49 -61.00-180.00   80
  7  \w     97.00 175.00   0.50    0.07    --  106.49  15.00-120.00  156
  8  \w    153.00 178.00   0.50    0.07    --  106.49  77.00  30.00   50
  9  \w    135.00 161.00   0.50    0.07    --  106.49  61.00  60.00   52
 10  \w     93.00 131.00   0.50    0.07    --  106.49  61.00  60.00   76
 11  \w    102.00 128.00   0.50    0.07    --  106.49  77.00  30.00   52
 12  \w     83.00 172.00   0.50    0.07    --  106.49  80.00 -51.00  178
 13  \w     48.00  73.00   0.50    0.05    --   47.45  80.00 -51.00   50
 14  \w     34.00  62.00   0.50    0.07    --  106.49 -61.00 -90.00   56
 15  \w     38.00  63.00   0.50    0.07    --  106.49 -61.00 -30.00   50
 16  \w     34.00  72.00   0.50    0.07    --  106.49 -94.00  30.00   76
 17  \w     38.00  74.00   0.50    0.07    --  106.49 -61.00   0.00   72
 18  \w     37.00  62.00   0.50    0.07    --  106.49 -61.00 120.00   50
 19  \w    -71.00  24.00   0.50    0.05    --  -47.45  80.00 -51.00  190
 20  \w    -40.00 -14.00   0.50    0.07    --  -86.25  45.00 150.00   52
 21  \w    -68.00 -21.00   0.50    0.07    --  -86.25  61.00 150.00   94
 22  \w    -85.00 -59.00   0.50    0.07    --  -86.25  80.00 -51.00   52
 23  \w   -115.00 -77.00   0.50    0.05    --  -47.45-125.00 -30.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1181929000
_diffrn_orient_matrix_UB_12      0.0338298000
_diffrn_orient_matrix_UB_13      -0.0694591000
_diffrn_orient_matrix_UB_21      -0.0410657000
_diffrn_orient_matrix_UB_22      0.0800397000
_diffrn_orient_matrix_UB_23      0.0522095000
_diffrn_orient_matrix_UB_31      0.1382559000
_diffrn_orient_matrix_UB_32      0.0526766000
_diffrn_orient_matrix_UB_33      -0.0346585000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13580
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.870
_diffrn_reflns_theta_min         3.964
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.019
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.496
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.012
_refine_diff_density_min         -1.233
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0494P)^2^+0.9532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3922
_reflns_number_total             4240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01463j2.cif
_cod_data_source_block           nh-34
_cod_depositor_comments          'Adding full bibliography for 7704579.cif.'
_cod_database_code               7704579
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C18H32N2O4Sn
_shelx_estimated_absorpt_t_max   0.434
_shelx_estimated_absorpt_t_min   0.289
_diffrn_oxdiff_ac4_digest_frames
;
01ea1d5671da5fe16deb314286e1015dda019083f5f
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C11(H11)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              66459
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.434
_oxdiff_exptl_absorpt_empirical_full_min 0.684