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_7708993
_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 Al Cl N2 O4'
_chemical_formula_sum            'C18 H32 Al Cl N2 O4'
_chemical_formula_weight         402.88
_chemical_name_systematic        L2AlCl
_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             2021-08-06
_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                 103.938(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1273(2)
_cell_length_b                   12.6240(2)
_cell_length_c                   14.5316(3)
_cell_measurement_reflns_used    20616
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.5220
_cell_measurement_theta_min      4.1940
_cell_volume                     2159.21(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_environment      N~2~
_diffrn_ambient_temperature      150.00(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 0.997
_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 -66.00 3.00 1.00 1.00 -- -42.62 38.00 90.00 69
 2 \w -85.00 -18.00 1.00 1.00 -- -42.62 -57.00-150.00 67
 3 \w -57.00 11.00 1.00 1.00 -- -42.62 38.00 150.00 68
 4 \w -82.00 36.00 1.00 1.00 -- -42.62 19.00 0.00 118
 5 \w -62.00 -14.00 1.00 1.00 -- -42.62 -57.00 120.00 48
 6 \w -103.00 -14.00 1.00 1.00 -- -42.62 -57.00 -60.00 89
 7 \w -116.00 -15.00 1.00 1.00 -- -42.62 -57.00 30.00 101
 8 \w -19.00 67.00 1.00 1.00 -- 42.62 -38.00 120.00 86
 9 \w 8.00 34.00 1.00 1.00 -- 42.62 83.00 116.17 26
 10 \w 8.00 34.00 1.00 1.00 -- 42.62 83.00-124.50 26
 11 \w 10.00 39.00 1.00 1.00 -- 42.62 79.00 152.66 29
 12 \w 15.00 42.00 1.00 1.00 -- 42.62 78.00 -19.77 27
 13 \w 10.00 35.00 1.00 1.00 -- 42.62 75.00 -46.24 25
 14 \w 44.00 97.00 1.00 1.00 -- 42.62-125.00 -90.00 53
 15 \w 11.00 36.00 1.00 1.00 -- 42.62 75.00 68.73 25
 16 \w 74.00 149.00 1.00 1.60 -- 104.49 68.00 -46.97 75
 17 \w 75.00 101.00 1.00 1.60 -- 104.49 63.00 80.74 26
 18 \w 73.00 99.00 1.00 1.60 -- 104.49 73.00-151.96 26
 19 \w 77.00 109.00 1.00 1.60 -- 104.49 56.00 -7.85 32
 20 \w 74.00 101.00 1.00 1.60 -- 104.49 72.00-116.66 27
 21 \w 133.00 176.00 1.00 1.60 -- 104.49 66.00-179.79 43
 22 \w 74.00 101.00 1.00 1.60 -- 104.49 66.00 134.97 27
 23 \w 75.00 109.00 1.00 1.60 -- 104.49 61.00 150.00 34
 24 \w 33.00 81.00 1.00 1.60 -- 104.49-125.00-150.00 48
 25 \w 83.00 113.00 1.00 1.60 -- 104.49-125.00-150.00 30
 26 \w 75.00 102.00 1.00 1.60 -- 104.49 61.00 120.00 27
 27 \w 27.00 104.00 1.00 1.60 -- 104.49 -94.00 -60.00 77
 28 \w 74.00 100.00 1.00 1.60 -- 104.49 67.00 65.34 26
 29 \w 74.00 101.00 1.00 1.60 -- 104.49 68.00 12.82 27
 30 \w 74.00 178.00 1.00 1.60 -- 104.49 68.00 98.12 104
 31 \w 136.00 162.00 1.00 1.60 -- 104.49 58.00 -65.38 26
 32 \w 74.00 100.00 1.00 1.60 -- 104.49 66.00-179.79 26
 33 \w 75.00 137.00 1.00 1.60 -- 104.49 61.00-127.92 62
 34 \w 97.00 164.00 1.00 1.60 -- 104.49 125.00-120.00 67
 35 \w 76.00 137.00 1.00 1.60 -- 104.49 61.00-112.09 61
 36 \w 77.00 122.00 1.00 1.60 -- 104.49 58.00 -65.38 45
 37 \w 75.00 102.00 1.00 1.60 -- 104.49 61.00 -90.00 27
 38 \w 76.00 102.00 1.00 1.60 -- 104.49 61.00 -60.00 26
 39 \w 33.00 113.00 1.00 1.60 -- 104.49-125.00 120.00 80
 40 \w 75.00 107.00 1.00 1.60 -- 104.49 61.00-150.00 32
 41 \w 22.00 102.00 1.00 1.60 -- 104.49 -94.00-120.00 80
 42 \w 75.00 102.00 1.00 1.60 -- 104.49 61.00 60.00 27
 43 \w 121.00 178.00 1.00 1.60 -- 104.49 72.00 117.37 57
 44 \w 116.00 174.00 1.00 1.60 -- 104.49 125.00 -60.00 58
 45 \w 23.00 87.00 1.00 1.60 -- 104.49 -94.00 30.00 64
 46 \w 75.00 117.00 1.00 1.60 -- 104.49 61.00 90.00 42
 47 \w 74.00 101.00 1.00 1.60 -- 104.49 72.00 117.37 27
 48 \w 153.00 178.00 1.00 1.60 -- 104.49 73.00-151.96 25
 49 \w 76.00 103.00 1.00 1.60 -- 104.49 61.00 -30.00 27
 50 \w 75.00 102.00 1.00 1.60 -- 104.49 61.00 30.00 27
 51 \w 75.00 154.00 1.00 1.60 -- 104.49 61.00 0.00 79
 52 \w 77.00 175.00 1.00 1.60 -- 104.49 57.00 44.24 98
 53 \w 77.00 146.00 1.00 1.60 -- 104.49 53.00 179.87 69
 54 \w 77.00 102.00 1.00 1.60 -- 104.49 58.00-158.08 25
;
_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      0.0669455000
_diffrn_orient_matrix_UB_12      0.1040513000
_diffrn_orient_matrix_UB_13      0.0022337000
_diffrn_orient_matrix_UB_21      0.1114893000
_diffrn_orient_matrix_UB_22      -0.0594465000
_diffrn_orient_matrix_UB_23      0.0429612000
_diffrn_orient_matrix_UB_31      0.0148597000
_diffrn_orient_matrix_UB_32      -0.0230480000
_diffrn_orient_matrix_UB_33      -0.1004075000
_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  0.0429
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34653
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.736
_diffrn_reflns_theta_min         4.274
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76765
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_preparation
'reaction of lithiated ligand with aluminium chloride'
_exptl_crystal_recrystallization_method 'crystallised from hexane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.252
_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     243
_refine_ls_number_reflns         4257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0559P)^2^+0.9733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3875
_reflns_number_total             4257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03365d2.cif
_cod_data_source_block           xstr1337
_cod_depositor_comments
'Adding full bibliography for 7708993--7708999.cif.'
_cod_database_code               7708993
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C72 H136 Al4 Cl4 N16 O8 '
_chemical_oxdiff_usercomment     'CEK KLM'
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.813
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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:
 C12(H12), C3(H3)
1.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C1(H1A,H1B,H1C), C9(H9A,H9B,H9C),
 C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              27558
_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 1.661
_oxdiff_exptl_absorpt_empirical_full_min 0.635