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_7708995
_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 Al Cl2 N O2'
_chemical_formula_sum            'C9 H16 Al Cl2 N O2'
_chemical_formula_weight         268.11
_chemical_name_systematic        'Aluminium dichloride isopropylamidoenoate'
_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
_audit_creation_date             2021-08-06
_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                 98.3700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.04510(10)
_cell_length_b                   8.10630(10)
_cell_length_c                   18.2392(2)
_cell_measurement_reflns_used    15491
_cell_measurement_temperature    150.00(1)
_cell_measurement_theta_max      73.1620
_cell_measurement_theta_min      4.9530
_cell_volume                     1323.10(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(1)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_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    -68.00 -23.00   1.00    1.00    --  -43.29 -38.00-120.00   45
  2  \w   -111.00 -17.00   1.00    1.00    --  -43.29 -57.00  60.00   94
  3  \w    -70.00  27.00   1.00    1.00    --  -43.29  57.00  90.00   97
  4  \w    -76.00 -17.00   1.00    1.00    --  -43.29 -57.00-150.00   59
  5  \w    -95.00 -18.00   1.00    1.00    --  -43.29 -57.00 150.00   77
  6  \w    -84.00 -17.00   1.00    1.00    --  -43.29 -57.00 -30.00   67
  7  \w    -85.00  -6.00   1.00    1.00    --  -43.29 125.00 150.00   79
  8  \w     12.00  37.00   1.00    1.00    --   43.29  78.00 -21.46   25
  9  \w    -29.00   7.00   1.00    1.00    --   43.29 -38.00 120.00   36
 10  \w     15.00  40.00   1.00    1.00    --   43.29  77.00   1.23   25
 11  \w     12.00  37.00   1.00    1.00    --   43.29  76.00 171.84   25
 12  \w     13.00  42.00   1.00    1.00    --   43.29  77.00  80.96   29
 13  \w     30.00  59.00   1.00    1.00    --   43.29 -38.00 120.00   29
 14  \w     11.00  36.00   1.00    1.00    --   43.29  79.00-155.84   25
 15  \w    -21.00  53.00   1.00    1.00    --   43.29 -77.00 -60.00   74
 16  \w     79.00 151.00   1.00    2.69    --  105.52  62.00 -20.32   72
 17  \w    127.00 175.00   1.00    2.69    --  105.52  65.00 116.25   48
 18  \w     76.00 175.00   1.00    2.69    --  105.52  70.00  12.15   99
 19  \w     77.00 103.00   1.00    2.69    --  105.52  65.00 116.25   26
 20  \w     78.00 105.00   1.00    2.69    --  105.52  61.00  60.00   27
 21  \w     77.00 114.00   1.00    2.69    --  105.52  64.00-163.96   37
 22  \w     81.00 112.00   1.00    2.69    --  105.52  47.00  97.67   31
 23  \w     78.00 113.00   1.00    2.69    --  105.52  61.00 -60.00   35
 24  \w    119.00 154.00   1.00    2.69    --  105.52  61.00  60.00   35
 25  \w     78.00 111.00   1.00    2.69    --  105.52  61.00 150.00   33
 26  \w    120.00 176.00   1.00    2.69    --  105.52  61.00 150.00   56
 27  \w     35.00  83.00   1.00    2.69    --  105.52 -77.00-120.00   48
 28  \w    106.00 136.00   1.00    2.69    --  105.52 -77.00-120.00   30
 29  \w    109.00 148.00   1.00    2.69    --  105.52  72.00-160.45   39
 30  \w     85.00 121.00   1.00    2.69    --  105.52  45.00 -30.00   36
 31  \w     79.00 104.00   1.00    2.69    --  105.52  61.00  90.00   25
 32  \w     92.00 137.00   1.00    2.69    --  105.52 -77.00  30.00   45
 33  \w     75.00 102.00   1.00    2.69    --  105.52  72.00-160.45   27
 34  \w     77.00 175.00   1.00    2.69    --  105.52  66.00-116.91   98
 35  \w    128.00 172.00   1.00    2.69    --  105.52  61.00 -90.00   44
 36  \w     33.00  77.00   1.00    2.69    --  105.52 -77.00  30.00   44
 37  \w     78.00 105.00   1.00    2.69    --  105.52  61.00 -90.00   27
 38  \w     25.00 106.00   1.00    2.69    --  105.52 -94.00 -60.00   81
 39  \w     81.00 143.00   1.00    2.69    --  105.52  45.00-120.00   62
 40  \w     78.00 105.00   1.00    2.69    --  105.52  61.00 -30.00   27
 41  \w     78.00 105.00   1.00    2.69    --  105.52  59.00 174.90   27
 42  \w    114.00 175.00   1.00    2.69    --  105.52  61.00  90.00   61
 43  \w     35.00 113.00   1.00    2.69    --  105.52-125.00 120.00   78
 44  \w    131.00 176.00   1.00    2.69    --  105.52  61.00 -60.00   45
 45  \w     81.00 108.00   1.00    2.69    --  105.52  45.00 120.00   27
 46  \w     34.00 113.00   1.00    2.69    --  105.52-125.00-120.00   79
 47  \w     79.00 106.00   1.00    2.69    --  105.52  61.00   0.00   27
 48  \w     76.00 102.00   1.00    2.69    --  105.52  68.00 -80.75   26
 49  \w     81.00 107.00   1.00    2.69    --  105.52  45.00  60.00   26
 50  \w     82.00 109.00   1.00    2.69    --  105.52  45.00  90.00   27
 51  \w     83.00 110.00   1.00    2.69    --  105.52  45.00 150.00   27
 52  \w     79.00 106.00   1.00    2.69    --  105.52  61.00-180.00   27
 53  \w     81.00 107.00   1.00    2.69    --  105.52  46.00-105.58   26
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Atlas diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0571555000
_diffrn_orient_matrix_UB_12      0.1761533000
_diffrn_orient_matrix_UB_13      -0.0106938000
_diffrn_orient_matrix_UB_21      0.0754659000
_diffrn_orient_matrix_UB_22      0.0024567000
_diffrn_orient_matrix_UB_23      0.0813540000
_diffrn_orient_matrix_UB_31      0.1438180000
_diffrn_orient_matrix_UB_32      -0.0712467000
_diffrn_orient_matrix_UB_33      -0.0235553000
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19674
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.463
_diffrn_reflns_theta_min         5.188
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.928
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_preparation       'Salt metathesis reaction'
_exptl_crystal_recrystallization_method 'recrystallised from hexane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0388P)^2^+0.4433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2561
_reflns_number_total             2631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03365d2.cif
_cod_data_source_block           xstr1295
_cod_depositor_comments
'Adding full bibliography for 7708993--7708999.cif.'
_cod_database_code               7708995
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C9H16AlO2NCl2
_chemical_oxdiff_usercomment     'CEK KLM'
_shelx_estimated_absorpt_t_max   0.639
_shelx_estimated_absorpt_t_min   0.439
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Ternary CH refined with riding coordinates:
 C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C4(H4A,H4B,H4C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              83625
_olex2_exptl_crystal_mounting_method
'using oil on a nylon loop under flow of N2'
_olex2_submission_original_sample_id AlCl2(AME)iPr
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.668
_oxdiff_exptl_absorpt_empirical_full_min 0.702