SnO via Water Based ALD employing Tin(II) Formamidinate: Precursor Characterization and Process Development
Huster, Niklas; Ghiyasi, Ramin; Zanders, David; Rogalla, Detlef; Karppinen, Maarit; Devi, Anjana; Dalton Transactions  (2022) –; doi:10.1039/D2DT02562K

data_7711100
_publ_section_title
;
 SnO via Water Based ALD employing Tin(II) Formamidinate: Precursor
 Characterization and Process Development
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02562K
_journal_year                    2022
_chemical_formula_moiety         'C16 H34 N4 Sn'
_chemical_formula_sum            'C16 H34 N4 Sn'
_chemical_formula_weight         401.16
_chemical_name_common            '[Sn(Et-tBu-AMD)2]'
_chemical_name_systematic        '[Sn(Et-tBu-AMD)2]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive,Oxygen-sensitive
_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             2019-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-05 deposited with the CCDC.	2022-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.756(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3446(3)
_cell_length_b                   10.1540(3)
_cell_length_c                   19.4816(7)
_cell_measurement_reflns_used    3120
_cell_measurement_temperature    99.97(18)
_cell_measurement_theta_max      73.1180
_cell_measurement_theta_min      4.3730
_cell_volume                     1987.63(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      99.97(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4409
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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    -88.00  38.00   1.00    2.50    --  -41.47  19.00 150.00  126
  2  \w     16.00  61.00   1.00    2.50    --   41.47-125.00 -60.00   45
  3  \w     33.00  60.00   1.00   10.00    --  108.47 -77.00 -60.00   27
  4  \w     43.00 137.00   1.00   10.00    --  108.47 -30.00  30.00   94
  5  \w    105.00 142.00   1.00   10.00    --  108.47 -77.00 -60.00   37
  6  \w     95.00 150.00   1.00   10.00    --  108.47  45.00-120.00   55
  7  \w     91.00 157.00   1.00   10.00    --  108.47  45.00-150.00   66
  8  \w     82.00 108.00   1.00   10.00    --  108.47  61.00-150.00   26
  9  \w     79.00 130.00   1.00   10.00    --  108.47  77.00 -90.00   51
 10  \w    106.00 132.00   1.00   10.00    --  108.47  45.00  60.00   26
 11  \w     91.00 158.00   1.00   10.00    --  108.47 125.00  90.00   67
 12  \w   -120.00 -79.00   1.00    2.50    --  -41.47 -99.00  30.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1494843000
_diffrn_orient_matrix_UB_12      -0.0333468000
_diffrn_orient_matrix_UB_13      0.0160838000
_diffrn_orient_matrix_UB_21      0.0255190000
_diffrn_orient_matrix_UB_22      0.0935569000
_diffrn_orient_matrix_UB_23      0.0641023000
_diffrn_orient_matrix_UB_31      -0.0226451000
_diffrn_orient_matrix_UB_32      -0.1147522000
_diffrn_orient_matrix_UB_33      0.0474878000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7525
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.786
_diffrn_reflns_theta_min         4.400
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.068
_refine_diff_density_max         2.028
_refine_diff_density_min         -2.109
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0816P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3298
_reflns_number_total             3910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02562k2.cif
_cod_data_source_block           nh-m8
_cod_database_code               7711100
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Sn1C8H17N2
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Secondary CH2 refined with riding coordinates:
 C008(H00A,H00B), C00F(H00O,H00P)
2.b Idealised Me refined as rotating group:
 C00A(H00C,H00D,H00E), C00B(H00F,H00G,H00H), C00D(H00I,H00J,H00K), C00E(H00L,
 H00M,H00N), C00G(H00Q,H00R,H00S), C00H(H00T,H00U,H00V), C00I(H00W,H00X,H00Y),
 C00J(H00Z,H,HA), C00K(H00,HB,HC), C00L(H0AA,HD,HE)
;
_shelx_res_checksum              74354
_shelx_hkl_checksum              16079
_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 1.834
_oxdiff_exptl_absorpt_empirical_full_min 0.695