Molecular engineering of Ga-ketoiminates: synthesis, structure and evaluation as precursors for the additive-free spin-coated deposition of gallium oxide thin films
O’Donoghue, Richard; Rahman, Shafiqur; Mallick, Bert; Winter, Manuela; Rogalla, Detlef; Becker, Hans-Werner; Devi, Anjana; New Journal of Chemistry 42 (2018) 3196–; doi:10.1039/C7NJ04334A

data_7056888
_publ_section_title
;
 Molecular engineering of Ga-ketoiminates: synthesis, structure and
 evaluation as precursors for the additive-free spin-coated deposition of
 gallium oxide thin films
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3196
_journal_paper_doi               10.1039/C7NJ04334A
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C12 H26 Ga N3 O'
_chemical_formula_sum            'C12 H26 Ga N3 O'
_chemical_formula_weight         298.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1q3hw6
_audit_creation_date             2017-09-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-26 deposited with the CCDC.
2017-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.544(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7637(2)
_cell_length_b                   14.6029(4)
_cell_length_c                   13.3304(4)
_cell_measurement_reflns_used    3755
_cell_measurement_temperature    101.3(2)
_cell_measurement_theta_max      75.1140
_cell_measurement_theta_min      4.5050
_cell_volume                     1490.38(7)
_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    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101.3(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4409
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_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      8.00  35.00   1.00    1.00    --  -40.78  77.00 -60.00   27
  2  \w    -32.00  65.00   1.00    1.00    --   40.78 -38.00-150.00   97
  3  \w     82.00 109.00   1.00    4.00    --  109.91 -94.00 -60.00   27
  4  \w     74.00 138.00   1.00    4.00    --  109.91 -77.00 -30.00   64
  5  \w     63.00 119.00   1.00    4.00    --  109.91-125.00 -90.00   56
  6  \w     37.00 121.00   1.00    4.00    --  109.91 -30.00  30.00   84
  7  \w     95.00 142.00   1.00    4.00    --  109.91  30.00 -60.00   47
  8  \w     88.00 158.00   1.00    4.00    --  109.91  77.00-150.00   70
  9  \w     60.00 158.00   1.00    4.00    --  109.91  15.00  30.00   98
 10  \w     91.00 117.00   1.00    4.00    --  109.91-125.00 120.00   26
 11  \w     43.00 136.00   1.00    4.00    --  109.91 -45.00 120.00   93
 12  \w     36.00  94.00   1.00    4.00    --  109.91 -94.00 150.00   58
 13  \w     -7.00  67.00   1.00    1.00    --   40.78 -77.00  90.00   74
 14  \w    -20.00  61.00   1.00    1.00    --   40.78 -57.00 150.00   81
 15  \w    -71.00 -44.00   1.00    1.00    --  -40.78  77.00 -60.00   27
 16  \w   -111.00 -15.00   1.00    1.00    --  -40.78 -57.00-120.00   96
 17  \w     38.00 138.00   1.00    4.00    --  109.91 -61.00-120.00  100
;
_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      0.1058013000
_diffrn_orient_matrix_UB_12      -0.0808209000
_diffrn_orient_matrix_UB_13      -0.0326202000
_diffrn_orient_matrix_UB_21      -0.1059124000
_diffrn_orient_matrix_UB_22      -0.0669731000
_diffrn_orient_matrix_UB_23      0.0551345000
_diffrn_orient_matrix_UB_31      -0.1343967000
_diffrn_orient_matrix_UB_32      -0.0106686000
_diffrn_orient_matrix_UB_33      -0.0981347000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9173
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.110
_diffrn_reflns_theta_min         4.526
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.445
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61898
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0370P)^2^+1.5086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2608
_reflns_number_total             3016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj04334a2.cif
_cod_data_source_block           ga
_cod_depositor_comments
'Adding full bibliography for 7056886--7056889.cif.'
_cod_database_code               7056888
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Ga C12H26 N3 O'
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.696
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C),
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C)
;
_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 1.432
_oxdiff_exptl_absorpt_empirical_full_min 0.629