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_7708999
_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         'C36 H52 Al Cl N2 O4'
_chemical_formula_sum            'C36 H52 Al Cl N2 O4'
_chemical_formula_weight         639.22
_chemical_name_systematic        xstr1155
_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             2021-03-09
_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                 96.8650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.90810(10)
_cell_length_b                   23.8108(2)
_cell_length_c                   16.8695(2)
_cell_measurement_reflns_used    27976
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.0850
_cell_measurement_theta_min      4.5040
_cell_volume                     3552.52(7)
_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_temperature      150.00(1)
_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 0.998
_diffrn_measured_fraction_theta_max 0.991
_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    -75.00 -17.00   1.00    1.95    --  -42.62 -57.00  90.00   58
  2  \w    -55.00 -22.00   1.00    1.95    --  -42.62 -38.00 150.00   33
  3  \w    -79.00 -18.00   1.00    1.95    --  -42.62 -57.00  30.00   61
  4  \w   -106.00 -58.00   1.00    1.95    --  -42.62 -38.00 150.00   48
  5  \w   -115.00 -22.00   1.00    1.95    --  -42.62 -38.00-150.00   93
  6  \w   -115.00 -15.00   1.00    1.95    --  -42.62 -57.00 -60.00  100
  7  \w    -86.00  -6.00   1.00    1.95    --  -42.62 125.00  60.00   80
  8  \w    -85.00  -8.00   1.00    1.95    --  -42.62 125.00 -30.00   77
  9  \w    -87.00  -7.00   1.00    1.95    --  -42.62 125.00 150.00   80
 10  \w    -65.00 -14.00   1.00    1.95    --  -42.62 -57.00 150.00   51
 11  \w    -67.00  32.00   1.00    1.95    --  -42.62  38.00 -30.00   99
 12  \w   -114.00 -21.00   1.00    1.95    --  -42.62 -38.00 -30.00   93
 13  \w      8.00  33.00   1.00    1.95    --   42.62  83.00 -66.59   25
 14  \w     10.00  40.00   1.00    1.95    --   42.62  79.00 -20.62   30
 15  \w     10.00  35.00   1.00    1.95    --   42.62  75.00  68.93   25
 16  \w      8.00  33.00   1.00    1.95    --   42.62  83.00 167.62   25
 17  \w      8.00  33.00   1.00    1.95    --   42.62  83.00  93.90   25
 18  \w     10.00  35.00   1.00    1.95    --   42.62  77.00-109.02   25
 19  \w     82.00 109.00   1.00    7.79    --  112.00  64.00-169.09   27
 20  \w     82.00 109.00   1.00    7.79    --  112.00  66.00 -55.94   27
 21  \w     83.00 110.00   1.00    7.79    --  112.00  60.00 160.79   27
 22  \w    153.00 178.00   1.00    7.79    --  112.00  47.00  38.28   25
 23  \w     80.00 178.00   1.00    7.79    --  112.00  73.00 117.43   98
 24  \w     81.00 178.00   1.00    7.79    --  112.00  74.00 -57.24   97
 25  \w     82.00 118.00   1.00    7.79    --  112.00  64.00 -83.87   36
 26  \w    121.00 155.00   1.00    7.79    --  112.00  64.00 -83.87   34
 27  \w     30.00 107.00   1.00    7.79    --  112.00 -94.00 -90.00   77
 28  \w     83.00 109.00   1.00    7.79    --  112.00  61.00  90.00   26
 29  \w    107.00 143.00   1.00    7.79    --  112.00 -77.00 -60.00   36
 30  \w     29.00 107.00   1.00    7.79    --  112.00 -94.00 150.00   78
 31  \w     86.00 124.00   1.00    7.79    --  112.00  47.00  38.28   38
 32  \w     82.00 111.00   1.00    7.79    --  112.00  65.00-144.35   29
 33  \w     84.00 110.00   1.00    7.79    --  112.00  57.00 -90.87   26
 34  \w     81.00 108.00   1.00    7.79    --  112.00  70.00 129.86   27
 35  \w     80.00 106.00   1.00    7.79    --  112.00  74.00  91.80   26
 36  \w    117.00 176.00   1.00    7.79    --  112.00  74.00 -34.27   59
 37  \w    132.00 178.00   1.00    7.79    --  112.00  57.00-177.03   46
 38  \w     83.00 117.00   1.00    7.79    --  112.00  61.00 -60.00   34
 39  \w     84.00 111.00   1.00    7.79    --  112.00  57.00-177.03   27
 40  \w     80.00 108.00   1.00    7.79    --  112.00  74.00 -34.27   28
 41  \w     86.00 131.00   1.00    7.79    --  112.00  45.00 -90.00   45
 42  \w     83.00 177.00   1.00    7.79    --  112.00  61.00  60.00   94
 43  \w     83.00 116.00   1.00    7.79    --  112.00  61.00-150.00   33
 44  \w    133.00 178.00   1.00    7.79    --  112.00  61.00-150.00   45
 45  \w     86.00 121.00   1.00    7.79    --  112.00  45.00  30.00   35
 46  \w     83.00 112.00   1.00    7.79    --  112.00  61.00 120.00   29
 47  \w     83.00 110.00   1.00    7.79    --  112.00  61.00  30.00   27
 48  \w     83.00 110.00   1.00    7.79    --  112.00  61.00 150.00   27
 49  \w     85.00 176.00   1.00    7.79    --  112.00  57.00  83.71   91
 50  \w     83.00 110.00   1.00    7.79    --  112.00  60.00  72.33   27
 51  \w     83.00 112.00   1.00    7.79    --  112.00  60.00-132.45   29
 52  \w     83.00 116.00   1.00    7.79    --  112.00  61.00-120.00   33
 53  \w    138.00 178.00   1.00    7.79    --  112.00  61.00-120.00   40
 54  \w     83.00 110.00   1.00    7.79    --  112.00  61.00 -30.00   27
 55  \w     83.00 114.00   1.00    7.79    --  112.00  61.00   0.00   31
 56  \w    135.00 178.00   1.00    7.79    --  112.00  61.00   0.00   43
 57  \w     82.00 107.00   1.00    7.79    --  112.00  73.00 -25.99   25
 58  \w     40.00  83.00   1.00    7.79    --  112.00 -77.00 -60.00   43
 59  \w     50.00 109.00   1.00    7.79    --  112.00-111.00  30.00   59
 60  \w     85.00 111.00   1.00    7.79    --  112.00  54.00 175.39   26
 61  \w     81.00 109.00   1.00    7.79    --  112.00-111.00-120.00   28
 62  \w     51.00  80.00   1.00    7.79    --  112.00-111.00-120.00   29
 63  \w     47.00 109.00   1.00    7.79    --  112.00-111.00 120.00   62
 64  \w    138.00 176.00   1.00    7.79    --  112.00  64.00-169.09   38
 65  \w    117.00 177.00   1.00    7.79    --  112.00  60.00 160.79   60
 66  \w     85.00 150.00   1.00    7.79    --  112.00  52.00  53.89   65
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            61929
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.371
_diffrn_reflns_theta_min         3.713
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.195
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_preparation
'reaction of aluminium chloride with lithium salt of ligand in hexane'
_exptl_crystal_recrystallization_method 'crystalised from hexane'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+1.6077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6632
_reflns_number_total             7384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03365d2.cif
_cod_data_source_block           xstr1155
_cod_depositor_comments
'Adding full bibliography for 7708993--7708999.cif.'
_cod_database_code               7708999
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.916
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C16(H16), C13(H13), C34(H34), C31(H31)
1.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C23(H23A,H23B)
1.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C10(H10), C9(H9), C21(H21), C29(H29), C28(H28), C27(H27)
1.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C24(H24A,H24B,
 H24C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C33(H33A,H33B,H33C), C32(H32A,
 H32B,H32C)
;
_shelx_res_checksum              64031
_olex2_exptl_crystal_mounting_method
'Using oil dried with lithium metal and mounted onto a nylon loop.'
_olex2_submission_original_sample_id AlCl(AME)Dip2
_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
;