Investigations into the structure, reactivity, and AACVD of aluminium and gallium amidoenoate complexes.
Mears, Kristian L.; Bhide, Malavika A.; Knapp, Caroline E.; Carmalt, Claire J.; Dalton transactions (Cambridge, England : 2003) 51 (2021) 156–167; doi:10.1039/d1dt03365d

data_7708996
_publ_section_title
;
 Investigations into the structure, reactivity, and AACVD of aluminium and
 gallium amidoenoate complexes.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              156
_journal_page_last               167
_journal_paper_doi               10.1039/d1dt03365d
_journal_volume                  51
_journal_year                    2021
_chemical_formula_moiety         'C18 H32 Cl Ga N2 O4'
_chemical_formula_sum            'C18 H32 Cl Ga N2 O4'
_chemical_formula_weight         445.62
_chemical_name_systematic        'Gallium chlorido bis-isopropylamidoenoate'
_chemical_properties_physical    Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-06 deposited with the CCDC.	2021-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.144(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1961(2)
_cell_length_b                   12.6013(2)
_cell_length_c                   14.5825(2)
_cell_measurement_reflns_used    24955
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.4170
_cell_measurement_theta_min      3.6710
_cell_volume                     2182.42(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_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    -73.00 -21.00   1.00    1.00    --  -43.42 -38.00  90.00   52
  2  \w   -106.00 -67.00   1.00    1.00    --  -43.42 -57.00 -60.00   39
  3  \w    -90.00 -64.00   1.00    1.00    --  -43.42 -77.00 120.00   26
  4  \w    -58.00 -12.00   1.00    1.00    --  -43.42 -77.00   0.00   46
  5  \w    -62.00  27.00   1.00    1.00    --  -43.42  57.00-150.00   89
  6  \w    -37.00 -12.00   1.00    1.00    --  -43.42 -77.00 120.00   25
  7  \w   -115.00 -12.00   1.00    1.00    --  -43.42 -77.00-150.00  103
  8  \w    -62.00 -17.00   1.00    1.00    --  -43.42 -57.00 -60.00   45
  9  \w    -85.00  -2.00   1.00    1.00    --  -43.42 125.00 -90.00   83
 10  \w   -117.00 -14.00   1.00    1.00    --  -43.42 -77.00  90.00  103
 11  \w    -49.00 -12.00   1.00    1.00    --  -43.42 -77.00 -90.00   37
 12  \w   -117.00 -74.00   1.00    1.00    --  -43.42 -77.00 -90.00   43
 13  \w      1.00  61.00   1.00    1.00    --   43.42 -99.00  90.00   60
 14  \w     74.00 100.00   1.00    1.00    --  105.83  77.00 -90.00   26
 15  \w     78.00 108.00   1.00    1.00    --  105.83  61.00 -90.00   30
 16  \w     78.00 176.00   1.00    1.00    --  105.83  61.00  30.00   98
 17  \w    124.00 150.00   1.00    1.00    --  105.83  77.00-180.00   26
 18  \w     74.00 100.00   1.00    1.00    --  105.83  77.00   0.00   26
 19  \w     74.00 100.00   1.00    1.00    --  105.83  77.00-180.00   26
 20  \w     27.00  99.00   1.00    1.00    --  105.83 -94.00  60.00   72
 21  \w     78.00 129.00   1.00    1.00    --  105.83  61.00-120.00   51
 22  \w     78.00 170.00   1.00    1.00    --  105.83  61.00 120.00   92
 23  \w     74.00 100.00   1.00    1.00    --  105.83  77.00 120.00   26
 24  \w     81.00 107.00   1.00    1.00    --  105.83 -94.00 -30.00   26
 25  \w     78.00 103.00   1.00    1.00    --  105.83  61.00-180.00   25
 26  \w     74.00  99.00   1.00    1.00    --  105.83  77.00 -60.00   25
 27  \w    129.00 177.00   1.00    1.00    --  105.83  77.00 -60.00   48
 28  \w     74.00 100.00   1.00    1.00    --  105.83  77.00-150.00   26
 29  \w     78.00 165.00   1.00    1.00    --  105.83  61.00 -30.00   87
 30  \w     79.00 105.00   1.00    1.00    --  105.83  61.00 150.00   26
 31  \w     36.00 118.00   1.00    1.00    --  105.83-125.00-120.00   82
 32  \w    151.00 176.00   1.00    1.00    --  105.83  61.00   0.00   25
 33  \w     74.00  99.00   1.00    1.00    --  105.83  77.00 -30.00   25
 34  \w    148.00 176.00   1.00    1.00    --  105.83  61.00-150.00   28
 35  \w     79.00 105.00   1.00    1.00    --  105.83  61.00   0.00   26
 36  \w    114.00 178.00   1.00    1.00    --  105.83  77.00-120.00   64
 37  \w     78.00 145.00   1.00    1.00    --  105.83  61.00-150.00   67
 38  \w     78.00 104.00   1.00    1.00    --  105.83  61.00  90.00   26
 39  \w    148.00 175.00   1.00    1.00    --  105.83  77.00  90.00   27
 40  \w     79.00 144.00   1.00    1.00    --  105.83  61.00 -60.00   65
 41  \w     74.00 100.00   1.00    1.00    --  105.83  77.00  30.00   26
 42  \w     74.00 100.00   1.00    1.00    --  105.83  77.00  90.00   26
 43  \w     78.00 104.00   1.00    1.00    --  105.83  61.00  60.00   26
 44  \w     74.00 177.00   1.00    1.00    --  105.83  77.00 150.00  103
 45  \w     74.00  99.00   1.00    1.00    --  105.83  77.00-120.00   25
 46  \w     37.00 135.00   1.00    1.00    --  105.83 -77.00-120.00   98
 47  \w     34.00 113.00   1.00    1.00    --  105.83-125.00-180.00   79
 48  \w     77.00 174.00   1.00    1.00    --  105.83  66.00  70.70   97
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1229068000
_diffrn_orient_matrix_UB_12      -0.0033235000
_diffrn_orient_matrix_UB_13      -0.0570051000
_diffrn_orient_matrix_UB_21      -0.0263093000
_diffrn_orient_matrix_UB_22      0.1003773000
_diffrn_orient_matrix_UB_23      0.0513807000
_diffrn_orient_matrix_UB_31      0.0320555000
_diffrn_orient_matrix_UB_32      0.0696735000
_diffrn_orient_matrix_UB_33      -0.0766937000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32986
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.674
_diffrn_reflns_theta_min         4.275
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.048
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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    1.356
_exptl_crystal_description       irregular
_exptl_crystal_F_000             936
_exptl_crystal_preparation
'reaction of gallium chloride with 2 equiv of lithium salt of ligand'
_exptl_crystal_recrystallization_method 'crystallised from hexane'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0300P)^2^+2.3575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4231
_reflns_number_total             4359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03365d2.cif
_cod_data_source_block           exp_1511
_cod_depositor_comments
'Adding full bibliography for 7708993--7708999.cif.'
_cod_database_code               7708996
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ga Cl C18 H32 O4 N2'
_chemical_oxdiff_usercomment     'CEK KLM'
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.610
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C16(H16), C7(H7)
1.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C14(H14A,H14B)
1.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C2(H2)
1.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C4(H4A,H4B,H4C), C9(H9A,H9B,H9C),
 C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C6(H6A,H6B,H6C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              83688
_olex2_date_sample_data_collection 2019-03-06
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_olex2_submission_original_sample_id xstr1007
_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 1.512
_oxdiff_exptl_absorpt_empirical_full_min 0.772