Systematic molecular engineering of Zn-ketoiminates for application as precursors in atomic layer depositions of zinc oxide.
O' Donoghue, Richard; Peeters, Daniel; Rogalla, Detlef; Becker, Hans-Werner; Rechmann, Julian; Henke, Sebastian; Winter, Manuela; Devi, Anjana; Dalton transactions (Cambridge, England : 2003) 45 (2016) 19012–19023; doi:10.1039/c6dt03571j

data_7041044
_publ_section_title
;
 Systematic molecular engineering of Zn-ketoiminates for application as
 precursors in atomic layer depositions of zinc oxide.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19012
_journal_page_last               19023
_journal_paper_doi               10.1039/c6dt03571j
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         '2(C8 H14 N O Zn0.5)'
_chemical_formula_sum            'C16 H28 N2 O2 Zn'
_chemical_formula_weight         345.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-09-05 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.823(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5697(5)
_cell_length_b                   5.67097(8)
_cell_length_c                   17.9276(4)
_cell_measurement_reflns_used    22063
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      76.2390
_cell_measurement_theta_min      4.0740
_cell_volume                     1732.21(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega -117.00  -15.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -38.0000  -60.0000 102

  2 omega -115.00  -12.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000  150.0000 103

  3 omega    2.00   99.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302 -125.0000   30.0000 97

  4 omega  -20.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302  -99.0000  120.0000 103

  5 omega    2.00   99.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302 -125.0000  -60.0000 97

  6 omega    3.00   29.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   91.0000  -66.6619 26

  7 omega   11.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   83.0000   40.4327 29

  8 omega   15.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   81.0000 -167.6133 31

  9 omega   15.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   81.0000  146.8368 31

 10 omega   19.00   45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   82.0000   46.4447 26

 11 omega   20.00   47.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   79.0000  -64.8785 27

 12 omega   20.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   80.0000  162.5944 26

 13 omega   19.00   45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   82.0000 -121.8530 26

 14 omega   25.00  136.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -33.2908 111

 15 omega   28.00  141.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000 -111.6591 113

 16 omega   28.00  141.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000   66.7477 113

 17 omega   33.00  144.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000  163.7476 111

 18 omega   36.00  149.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000   -1.6474 113

 19 omega   36.00  149.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000  154.2474 113

 20 omega   34.00  147.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000    0.0000 113

 21 omega   79.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   60.0000 79

 22 omega   79.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  120.0000 79

 23 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -180.0000 75

 24 omega   38.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -150.0000 39

 25 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   90.0000 75

 26 omega   79.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -30.0000 79

 27 omega   38.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000    0.0000 39

 28 omega   79.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -120.0000 79

 29 omega   79.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   30.0000 79

 30 omega   79.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  150.0000 79

 31 omega   79.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -180.0000 79

 32 omega   35.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000    0.0000 81

 33 omega   79.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -150.0000 79

 34 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -60.0000 75

 35 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -30.0000 75

 36 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   60.0000 75

 37 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  150.0000 75

 38 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  120.0000 75

 39 omega   35.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -180.0000 81

 40 omega   79.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   90.0000 79

 41 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -90.0000 75

 42 omega   79.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000    0.0000 79

 43 omega   35.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  -30.0000 81

 44 omega   35.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -180.0000 34

 45 omega   35.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   60.0000 34

 46 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -120.0000 75

 47 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -150.0000 75

 48 omega   29.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000 -150.0000 80

 49 omega   79.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -60.0000 79

 50 omega   38.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   30.0000 39

 51 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   30.0000 75

 52 omega   79.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -90.0000 79

 53 omega  -48.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302    0.0000   90.0000 179

 54 omega    8.00  120.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302   77.0000  120.0000 112

 55 omega  -48.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302    0.0000 -120.0000 179

 56 omega  -48.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302    0.0000  120.0000 179

 57 omega    2.00   99.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302 -125.0000   60.0000 97

 58 omega   15.00  117.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302   38.0000  -60.0000 102

 59 omega  -48.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302    0.0000 -180.0000 179

 60 omega   -5.00  123.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302   19.0000 -180.0000 128

 61 omega  -48.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302    0.0000 -150.0000 179

 62 omega  -48.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302    0.0000  -90.0000 179

 63 omega  -48.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302    0.0000  -60.0000 179

 64 omega  -48.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302    0.0000  -30.0000 179

 65 omega  -48.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302    0.0000    0.0000 179

 66 omega  -48.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302    0.0000   30.0000 179

 67 omega  -48.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302    0.0000   60.0000 179

 68 omega    4.00   33.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   89.0000 -139.9244 29

 69 omega   29.00  140.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   38.6144 111

 70 omega   29.00  140.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  -15.5500 111

 71 omega   85.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  150.0000 73

 72 omega   85.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   60.0000 73

 73 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000    0.0000 75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0544368000
_diffrn_orient_matrix_UB_12      0.0268782000
_diffrn_orient_matrix_UB_13      0.1082606000
_diffrn_orient_matrix_UB_21      -0.0628267000
_diffrn_orient_matrix_UB_22      0.1505305000
_diffrn_orient_matrix_UB_23      -0.0069739000
_diffrn_orient_matrix_UB_31      -0.0355997000
_diffrn_orient_matrix_UB_32      -0.2245551000
_diffrn_orient_matrix_UB_33      0.0082849000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31521
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.170
_diffrn_reflns_theta_min         4.100
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.009
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       plank
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.0664
_exptl_crystal_size_min          0.0437
_refine_diff_density_max         1.225
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 1539 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.202(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3572
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0720P)^2^+1.5290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                3524
_reflns_number_total             3572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03571j2.cif
_cod_data_source_block           cvd488_red_c2
_cod_depositor_comments
'Adding full bibliography for 7041043--7041046.cif.'
_cod_original_cell_volume        1732.20(10)
_cod_database_code               7041044
_chemical_oxdiff_formula         'Zn C16 H28 N2 O2'
_reflns_odcompleteness_completeness 99.94
_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), C14(H14A,H14B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,
 H13B,H13C), C16(H16A,H16B,H16C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'