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_7056889
_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         'C27 H48 Ga N3 O6'
_chemical_formula_sum            'C27 H48 Ga N3 O6'
_chemical_formula_weight         580.40
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1q3hx7
_audit_creation_date             2017-08-21
_audit_creation_method
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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                 122.791(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4543(4)
_cell_length_b                   8.65960(10)
_cell_length_c                   22.4511(9)
_cell_measurement_reflns_used    6085
_cell_measurement_temperature    111.1(3)
_cell_measurement_theta_max      76.2040
_cell_measurement_theta_min      5.0430
_cell_volume                     3016.12(16)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      111.1(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
  1 omega -116.00  -80.00   1.0000    5.1850
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -99.0000  -30.0000 36

  2 omega -113.00  -84.00   1.0000    5.1850
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -99.0000   30.0000 29

  3 omega  -29.00   68.00   1.0000    5.1850
omega____ theta____ kappa____ phi______ frames
    -       41.2302  -57.0000 -120.0000 97

  4 omega   17.00  111.00   1.0000    5.1850
omega____ theta____ kappa____ phi______ frames
    -       41.2302   57.0000   30.0000 94

  5 omega  108.00  144.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   90.0000 36

  6 omega   46.00   77.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  150.0000 31

  7 omega   38.00   77.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -180.0000 39

  8 omega   36.00   69.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   60.0000 33

  9 omega   35.00   69.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   90.0000 34

 10 omega   35.00   94.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000   60.0000 59

 11 omega   30.00   58.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000  120.0000 28

 12 omega   39.00   69.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 30

 13 omega   40.00   92.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   60.0000 52

 14 omega  109.00  135.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   60.0000 26

 15 omega   35.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000   90.0000 81

 16 omega   92.00  138.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000  120.0000 46

 17 omega   51.00  103.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000  150.0000 52
;
_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      -0.0812117000
_diffrn_orient_matrix_UB_12      0.0509781000
_diffrn_orient_matrix_UB_13      -0.0038044000
_diffrn_orient_matrix_UB_21      0.0252159000
_diffrn_orient_matrix_UB_22      0.0108726000
_diffrn_orient_matrix_UB_23      0.0814470000
_diffrn_orient_matrix_UB_31      0.0227069000
_diffrn_orient_matrix_UB_32      0.1700379000
_diffrn_orient_matrix_UB_33      -0.0039773000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13120
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.332
_diffrn_reflns_theta_min         3.950
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91007
_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    1.278
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0311
_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^+1.2047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5425
_reflns_number_total             6196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj04334a2.cif
_cod_data_source_block           rod-013i
_cod_depositor_comments
'Adding full bibliography for 7056886--7056889.cif.'
_cod_original_cell_volume        3016.12(15)
_cod_database_code               7056889
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Ga2 C50 H100 O6 N3'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12), C21(H21)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C23(H23A,H23B,
 H23C), C27(H27A,H27B,H27C)
;
_olex2_submission_special_instructions 'No special instructions were received'