Synthesis and characterisation of novel aluminium and gallium precursors for chemical vapour deposition
Knapp, Caroline E.; Marchand, Peter; Dyer, Caragh; Parkin, Ivan P.; Carmalt, Claire J.; New J. Chem. 39 (2015) 6585–; doi:10.1039/C5NJ00947B

data_7054959
_publ_section_title
;
 Synthesis and characterisation of novel aluminium and gallium precursors
 for chemical vapour deposition
;
_journal_issue                   8
_journal_name_full               'New J. Chem.'
_journal_page_first              6585
_journal_paper_doi               10.1039/C5NJ00947B
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C23 H25 Ga N2 O2'
_chemical_formula_sum            'C23 H25 Ga N2 O2'
_chemical_formula_weight         431.17
_chemical_name_systematic        'Methylgallium betadiketonate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-17 deposited with the CCDC.
2015-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4044(4)
_cell_length_b                   13.0468(6)
_cell_length_c                   21.5066(11)
_cell_measurement_reflns_used    4670
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.0590
_cell_measurement_theta_min      4.1200
_cell_volume                     2077.62(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_temperature      100.00(10)
_diffrn_detector_area_resol_mean 5.2031
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details
;
  1 omega   -2.00   30.00   1.0000    3.2700
omega____ theta____ kappa____ phi______ frames
    -      -10.9772  -19.0000 -120.0000 32

  2 omega  -52.00  -19.00   1.0000    3.2700
omega____ theta____ kappa____ phi______ frames
    -      -10.9772  -19.0000 -120.0000 33

  3 omega  -75.00  -34.00   1.0000    3.2700
omega____ theta____ kappa____ phi______ frames
    -      -10.9772  -38.0000   60.0000 41

  4 omega  -14.00   13.00   1.0000    3.2700
omega____ theta____ kappa____ phi______ frames
    -      -10.9772  -38.0000   60.0000 27

  5 omega   49.00   94.00   1.0000    3.2700
omega____ theta____ kappa____ phi______ frames
    -       12.0709 -178.0000 -120.0000 45
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0704226000
_diffrn_orient_matrix_UB_12      -0.0318676000
_diffrn_orient_matrix_UB_13      -0.0113338000
_diffrn_orient_matrix_UB_21      -0.0213416000
_diffrn_orient_matrix_UB_22      0.0372305000
_diffrn_orient_matrix_UB_23      -0.0228643000
_diffrn_orient_matrix_UB_31      0.0614371000
_diffrn_orient_matrix_UB_32      -0.0234315000
_diffrn_orient_matrix_UB_33      -0.0208974000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9421
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.290
_diffrn_reflns_theta_min         3.123
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.345
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_preparation
'Reaction of betadiketonate with trimethylgallium'
_exptl_crystal_recrystallization_method 'Crystallised from hexane'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 1493 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0314P)^2^+0.3175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.590
_reflns_friedel_fraction_full    0.867
_reflns_friedel_fraction_max     0.692
_reflns_number_gt                4284
_reflns_number_total             4574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00947b1.cif
_cod_data_source_block           xstr0104
_cod_depositor_comments
'Adding full bibliography for 7054959--7054961.cif.'
_cod_original_cell_volume        2077.61(18)
_cod_database_code               7054959
_chemical_oxdiff_formula         'Ga C23 H25 O2 N2'
_chemical_oxdiff_usercomment     'CEK Pete'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C2(H2B,H2A), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              36420
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2013-12-19
_olex2_exptl_crystal_mounting_method 'Mounted on a nylon loop'
_olex2_submission_original_sample_id XSTR0104
_olex2_submission_special_instructions 'No special instructions were received'