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_7056887
_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         'C20 H36 Cl Ga N2 O4'
_chemical_formula_sum            'C20 H36 Cl Ga N2 O4'
_chemical_formula_weight         473.68
_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     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc1q3hv5
_audit_creation_date             2017-09-27
_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                 91.153(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6212(2)
_cell_length_b                   13.9767(3)
_cell_length_c                   17.2781(5)
_cell_measurement_reflns_used    9006
_cell_measurement_temperature    99.8(2)
_cell_measurement_theta_max      74.0800
_cell_measurement_theta_min      4.0420
_cell_volume                     2322.96(10)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.8(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 0.985
_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   -117.00 -18.00   1.00    5.00    --  -42.53 -38.00 -90.00   99
  2  \w    -67.00  32.00   1.00    5.00    --  -42.53  38.00 120.00   99
  3  \w   -115.00 -14.00   1.00    5.00    --  -42.53 -57.00  30.00  101
  4  \w      2.00  99.00   1.00    5.00    --   42.53-125.00 -90.00   97
  5  \w     76.00 158.00   1.00   20.00    --  108.66  77.00   0.00   82
  6  \w     26.00 108.00   1.00   20.00    --  108.66 -94.00  60.00   82
  7  \w     33.00 141.00   1.00   20.00    --  108.66 -77.00 120.00  108
  8  \w     36.00 134.00   1.00   20.00    --  108.66 -45.00-150.00   98
  9  \w     73.00 158.00   1.00   20.00    --  108.66 125.00  90.00   85
 10  \w     80.00 158.00   1.00   20.00    --  108.66  61.00 -90.00   78
 11  \w   -119.00 -10.00   1.00    5.00    --  -42.53 -77.00 120.00  109
 12  \w   -119.00 -10.00   1.00    5.00    --  -42.53 -77.00-120.00  109
 13  \w   -115.00 -14.00   1.00    5.00    --  -42.53 -57.00 150.00  101
 14  \w     83.00 158.00   1.00   20.00    --  108.66  45.00 -30.00   75
 15  \w     80.00 158.00   1.00   20.00    --  108.66  30.00  90.00   78
 16  \w     80.00 158.00   1.00   20.00    --  108.66  61.00-120.00   78
 17  \w     35.00 122.00   1.00   20.00    --  108.66-125.00  60.00   87
 18  \w     80.00 158.00   1.00   20.00    --  108.66  30.00-150.00   78
;
_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      0.1572202000
_diffrn_orient_matrix_UB_12      0.0133352000
_diffrn_orient_matrix_UB_13      0.0149962000
_diffrn_orient_matrix_UB_21      -0.0025452000
_diffrn_orient_matrix_UB_22      -0.0794312000
_diffrn_orient_matrix_UB_23      0.0618232000
_diffrn_orient_matrix_UB_31      0.0304883000
_diffrn_orient_matrix_UB_32      -0.0753778000
_diffrn_orient_matrix_UB_33      -0.0623867000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21962
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.675
_diffrn_reflns_theta_min         4.069
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.895
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.523
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.354
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0430P)^2^+0.9491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3967
_reflns_number_total             4686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj04334a2.cif
_cod_data_source_block           cvd525f
_cod_depositor_comments
'Adding full bibliography for 7056886--7056889.cif.'
_cod_database_code               7056887
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Ga1 C20 H36 N2 O4'
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.487
_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) 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), C9(H9A,H9B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C15(H15A,H15B,H15C), C20(H20A,H20B,H20C)
;
_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 1.517
_oxdiff_exptl_absorpt_empirical_full_min 0.800