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_7708994
_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         'C9 H16 Cl2 Ga N O2'
_chemical_formula_sum            'C9 H16 Cl2 Ga N O2'
_chemical_formula_weight         310.85
_chemical_properties_physical    Air-sensitive,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     direct
_audit_creation_date             2021-03-09
_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                 98.2836(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.08077(15)
_cell_length_b                   8.02118(10)
_cell_length_c                   18.3319(3)
_cell_measurement_reflns_used    19522
_cell_measurement_temperature    151.6(4)
_cell_measurement_theta_max      73.5080
_cell_measurement_theta_min      4.8320
_cell_volume                     1321.34(4)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      151.6(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4061
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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 -12.00   1.00    1.00    --  -43.29 -77.00  60.00  105
  2  \w   -113.00 -17.00   1.00    1.00    --  -43.29 -57.00 -60.00   96
  3  \w   -117.00 -12.00   1.00    1.00    --  -43.29 -77.00 -90.00  105
  4  \w   -117.00 -12.00   1.00    1.00    --  -43.29 -77.00   0.00  105
  5  \w    -70.00  27.00   1.00    1.00    --  -43.29  57.00  90.00   97
  6  \w   -117.00 -12.00   1.00    1.00    --  -43.29 -77.00 150.00  105
  7  \w   -117.00 -12.00   1.00    1.00    --  -43.29 -77.00-180.00  105
  8  \w   -122.00  -6.00   1.00    1.00    --  -43.29 -19.00  60.00  116
  9  \w      1.00  83.00   1.00    1.00    --   43.29 -99.00-150.00   82
 10  \w      1.00  83.00   1.00    1.00    --   43.29 -99.00 -60.00   82
 11  \w     74.00 178.00   1.00    1.96    --  105.82  77.00 -60.00  104
 12  \w     74.00 178.00   1.00    1.96    --  105.82  77.00 120.00  104
 13  \w     78.00 176.00   1.00    1.96    --  105.82  61.00  30.00   98
 14  \w     74.00 178.00   1.00    1.96    --  105.82  77.00-120.00  104
 15  \w     94.00 177.00   1.00    1.96    --  105.82 125.00 120.00   83
 16  \w     78.00 176.00   1.00    1.96    --  105.82  61.00   0.00   98
 17  \w     77.00 177.00   1.00    1.96    --  105.82  67.00  39.34  100
 18  \w     74.00 178.00   1.00    1.96    --  105.82  77.00  90.00  104
 19  \w     25.00 109.00   1.00    1.96    --  105.82 -95.00 -90.00   84
 20  \w     74.00 178.00   1.00    1.96    --  105.82  77.00-150.00  104
 21  \w     74.00 178.00   1.00    1.96    --  105.82  77.00 -90.00  104
 22  \w     74.00 178.00   1.00    1.96    --  105.82  77.00 -30.00  104
 23  \w     78.00 176.00   1.00    1.96    --  105.82  61.00  60.00   98
 24  \w     78.00 176.00   1.00    1.96    --  105.82  61.00 -30.00   98
 25  \w     25.00 109.00   1.00    1.96    --  105.82 -95.00 150.00   84
 26  \w     78.00 176.00   1.00    1.96    --  105.82  61.00 -90.00   98
 27  \w     74.00 178.00   1.00    1.96    --  105.82  77.00   0.00  104
 28  \w     78.00 176.00   1.00    1.96    --  105.82  61.00-180.00   98
 29  \w     78.00 176.00   1.00    1.96    --  105.82  61.00 -60.00   98
 30  \w     78.00 176.00   1.00    1.96    --  105.82  61.00  90.00   98
 31  \w     78.00 176.00   1.00    1.96    --  105.82  61.00 150.00   98
 32  \w     25.00 109.00   1.00    1.96    --  105.82 -95.00  60.00   84
 33  \w     78.00 176.00   1.00    1.96    --  105.82  61.00-150.00   98
 34  \w     74.00 178.00   1.00    1.96    --  105.82  77.00-180.00  104
 35  \w     82.00 177.00   1.00    1.96    --  105.82  45.00   0.00   95
 36  \w     78.00 176.00   1.00    1.96    --  105.82  61.00-120.00   98
 37  \w     25.00 109.00   1.00    1.96    --  105.82 -95.00-150.00   84
 38  \w     78.00 176.00   1.00    1.96    --  105.82  63.00  66.60   98
 39  \w     76.00 177.00   1.00    1.96    --  105.82  69.00 154.53  101
 40  \w     74.00 178.00   1.00    1.96    --  105.82  77.00  60.00  104
 41  \w     77.00 177.00   1.00    1.96    --  105.82  66.00 117.97  100
 42  \w   -113.00 -17.00   1.00    1.00    --  -43.29 -57.00  90.00   96
 43  \w   -116.00 -21.00   1.00    1.00    --  -43.29 -38.00  60.00   95
 44  \w   -116.00 -21.00   1.00    1.00    --  -43.29 -38.00 -60.00   95
 45  \w   -113.00 -17.00   1.00    1.00    --  -43.29 -57.00-180.00   96
 46  \w   -113.00 -17.00   1.00    1.00    --  -43.29 -57.00  60.00   96
 47  \w    -43.00 130.00   1.00    1.00    --   43.29   0.00-180.00  173
 48  \w    -43.00  99.00   1.00    1.00    --   43.29   0.00 -30.00  142
 49  \w     12.00 117.00   1.00    1.00    --   43.29  77.00  60.00  105
 50  \w    -43.00 130.00   1.00    1.00    --   43.29   0.00 -60.00  173
 51  \w    -43.00 130.00   1.00    1.00    --   43.29   0.00 -90.00  173
 52  \w    -43.00 130.00   1.00    1.00    --   43.29   0.00-120.00  173
 53  \w    -43.00 130.00   1.00    1.00    --   43.29   0.00-150.00  173
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0021932000
_diffrn_orient_matrix_UB_12      -0.1910701000
_diffrn_orient_matrix_UB_13      0.0084209000
_diffrn_orient_matrix_UB_21      -0.0874040000
_diffrn_orient_matrix_UB_22      0.0180764000
_diffrn_orient_matrix_UB_23      0.0656424000
_diffrn_orient_matrix_UB_31      -0.1474069000
_diffrn_orient_matrix_UB_32      -0.0078872000
_diffrn_orient_matrix_UB_33      -0.0532363000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44799
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.794
_diffrn_reflns_theta_min         4.876
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.563
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_preparation
'stirred solution of lithiated ligand with one equivalent of gallium chloride in toluene'
_exptl_crystal_recrystallization_method 'crystallised from toluene'
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0316P)^2^+0.5774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2444
_reflns_number_total             2646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03365d2.cif
_cod_data_source_block           xstr0873
_cod_depositor_comments
'Adding full bibliography for 7708993--7708999.cif.'
_cod_original_cell_volume        1321.34(3)
_cod_database_code               7708994
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cl2 Ga N O2 C9 H16'
_chemical_oxdiff_usercomment     'CEK KLM'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C7(H7)
1.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
1.c Aromatic/amide H refined with riding coordinates:
 C2(H2)
1.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              92423
_olex2_date_sample_data_collection 2018-06-19
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_olex2_submission_original_sample_id xstr0873
_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 1.702
_oxdiff_exptl_absorpt_empirical_full_min 0.701