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_7054960
_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         'C16 H28 Cl Ga N2 O2'
_chemical_formula_sum            'C16 H28 Cl Ga N2 O2'
_chemical_formula_weight         385.57
_chemical_name_systematic
'chloro gallium bis(2-N-isopropylaminopentan-4-one)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-02-19
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;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-19 deposited with the CCDC.
2015-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.242(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3771(3)
_cell_length_b                   11.4009(3)
_cell_length_c                   14.2678(4)
_cell_measurement_temperature    150
_cell_volume                     1842.92(9)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_details
;
  1 omega    2.00   62.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2220 -112.0000  109.1803 60

  2 omega  -20.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2220   77.0000  120.0000 109

  3 omega  -14.00   81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2220   38.0000   30.0000 95

  4 omega  -20.00   54.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2220  -99.0000  -30.0000 74

  5 omega  -49.00   42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2220  -57.0000 -150.0000 91

  6 omega  -31.00   92.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2220   19.0000  -60.0000 123

  7 omega   11.00   71.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2220 -127.0000 -137.7590 60
;
_diffrn_orient_matrix_UB_11      0.0438775000
_diffrn_orient_matrix_UB_12      -0.0443487000
_diffrn_orient_matrix_UB_13      0.0044533000
_diffrn_orient_matrix_UB_21      0.0156559000
_diffrn_orient_matrix_UB_22      0.0174042000
_diffrn_orient_matrix_UB_23      0.0472456000
_diffrn_orient_matrix_UB_31      -0.0417845000
_diffrn_orient_matrix_UB_32      -0.0400027000
_diffrn_orient_matrix_UB_33      0.0155747000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_laue_measured_fraction_full 0.989
_diffrn_reflns_laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14260
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.325
_diffrn_reflns_theta_min         2.992
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.646
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81120
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_preparation       'Reaction of GaCl3 with 2 KL'
_exptl_crystal_recrystallization_method 'Grown from toluene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0360P)^2^+1.0490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2150
_reflns_number_total             2360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00947b1.cif
_cod_data_source_block           xstr0139
_cod_depositor_comments
'Adding full bibliography for 7054959--7054961.cif.'
_cod_original_cell_volume        1842.93(9)
_cod_database_code               7054960
_chemical_oxdiff_formula         'Ga N2 O2 C16 H28'
_chemical_oxdiff_usercomment     'CEK Caragh'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              31175
_shelx_shelxl_version_number     2014/7
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_date_sample_data_collection 2014-02-12
_olex2_date_sample_submission    1392214982.0
_olex2_exptl_crystal_mounting_method 'Nylon loop'
_olex2_submission_original_sample_id XSTR0139
_olex2_submission_special_instructions 'No special instructions were received'