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_7041045
_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_formula_moiety         'C18 H32 N2 O4 Zn'
_chemical_formula_sum            'C18 H32 N2 O4 Zn'
_chemical_formula_weight         405.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-05 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.615(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2557(4)
_cell_length_b                   5.89050(10)
_cell_length_c                   13.9479(6)
_cell_measurement_reflns_used    4927
_cell_measurement_temperature    105.5(8)
_cell_measurement_theta_max      73.8320
_cell_measurement_theta_min      5.4450
_cell_volume                     1043.62(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -99.00   -2.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  125.0000 -120.0000 97

  2 omega -124.00  -79.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -99.0000  -60.0000 45

  3 omega   15.00  117.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302   38.0000 -180.0000 102

  4 omega   34.00  139.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -61.0000 -180.0000 105

  5 omega   34.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000  120.0000 43

  6 omega   31.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000 -180.0000 38

  7 omega   24.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -94.0000  150.0000 85

  8 omega   34.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000  -30.0000 43

  9 omega   75.00  158.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000  -30.0000 83

 10 omega   73.00  158.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  125.0000 -150.0000 85

 11 omega -115.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000   60.0000 103

 12 omega -115.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000 -150.0000 103

 13 omega -115.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000  -30.0000 103

 14 omega   75.00  158.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000  -90.0000 83

 15 omega   81.00  158.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   45.0000   60.0000 77

 16 omega   81.00  158.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   45.0000 -150.0000 77

 17 omega   24.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -94.0000    0.0000 85

 18 omega   81.00  158.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   45.0000  150.0000 77
;
_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      -0.0642454000
_diffrn_orient_matrix_UB_12      0.1019541000
_diffrn_orient_matrix_UB_13      -0.1006383000
_diffrn_orient_matrix_UB_21      -0.0172689000
_diffrn_orient_matrix_UB_22      0.2181866000
_diffrn_orient_matrix_UB_23      0.0541045000
_diffrn_orient_matrix_UB_31      0.1014092000
_diffrn_orient_matrix_UB_32      0.1019867000
_diffrn_orient_matrix_UB_33      -0.0151414000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7792
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.061
_diffrn_reflns_theta_min         4.058
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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    1.291
_exptl_crystal_description       prism
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0459P)^2^+0.5225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2018
_reflns_number_total             2093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03571j2.cif
_cod_data_source_block           001
_cod_depositor_comments
'Adding full bibliography for 7041043--7041046.cif.'
_cod_database_code               7041045
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.71
_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)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              58875
_olex2_submission_special_instructions 'No special instructions were received'