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_7708998
_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 H53 Al N2 O4'
_chemical_formula_sum            'C36 H53 Al N2 O4'
_chemical_formula_weight         604.78
_chemical_name_systematic
'Aluminium hydrido bis-2,6-diisopropylphenylamidoenoate'
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.07670(10)
_cell_length_b                   21.07670(10)
_cell_length_c                   16.37980(10)
_cell_measurement_reflns_used    46371
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.5940
_cell_measurement_theta_min      5.3590
_cell_volume                     7276.35(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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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 -4.00 21.00 1.00 1.00 -- 34.00 92.00 -61.34 25
 2 \w 10.00 36.00 1.00 1.00 -- 42.00 75.00 88.51 26
 3 \w 7.00 32.00 1.00 1.00 -- 42.00 84.00 -41.92 25
 4 \w 10.00 35.00 1.00 1.00 -- 42.00 75.00-107.88 25
 5 \w 7.00 33.00 1.00 1.00 -- 42.00 84.00 79.38 26
 6 \w -86.00 -6.00 1.00 1.00 -- -42.87 125.00 60.00 80
 7 \w -113.00 -18.00 1.00 1.00 -- -42.87 -38.00 0.00 95
 8 \w -70.00 28.00 1.00 1.00 -- -42.87 57.00 -30.00 98
 9 \w -112.00 -22.00 1.00 1.00 -- -42.87 -38.00 -90.00 90
 10 \w -98.00 -18.00 1.00 1.00 -- -42.87 -38.00 150.00 80
 11 \w 13.00 38.00 1.00 1.00 -- 46.00 79.00 169.87 25
 12 \w 14.00 42.00 1.00 1.00 -- 46.00 79.00 5.81 28
 13 \w 27.00 54.00 1.00 1.00 -- 58.00 72.00-106.26 27
 14 \w 30.00 57.00 1.00 1.00 -- 62.00 74.00 -80.13 27
 15 \w 107.00 135.00 1.00 1.00 -- 66.00 73.00 17.64 28
 16 \w 34.00 60.00 1.00 1.00 -- 66.00 73.00 159.99 26
 17 \w 34.00 61.00 1.00 1.00 -- 66.00 73.00-160.90 27
 18 \w 34.00 61.00 1.00 1.00 -- 66.00 73.00 17.64 27
 19 \w 35.00 61.00 1.00 1.00 -- 66.00 72.00 100.71 26
 20 \w 39.00 64.00 1.00 1.00 -- 70.00 74.00 -51.03 25
 21 \w 39.00 64.00 1.00 1.00 -- 70.00 74.00 -22.14 25
 22 \w 113.00 143.00 1.00 1.00 -- 70.00 74.00 -51.03 30
 23 \w 39.00 66.00 1.00 1.00 -- 70.00 74.00 36.79 27
 24 \w 39.00 81.00 1.00 1.00 -- 70.00 73.00 109.75 42
 25 \w 46.00 72.00 1.00 1.49 -- 74.00 67.00 155.16 26
 26 \w 43.00 68.00 1.00 1.49 -- 74.00 74.00 -69.98 25
 27 \w 42.00 70.00 1.00 1.49 -- 74.00 74.00 56.73 28
 28 \w 50.00 76.00 1.00 1.49 -- 82.00 73.00 -17.21 26
 29 \w 50.00 76.00 1.00 1.49 -- 82.00 74.00-150.49 26
 30 \w 105.00 155.00 1.00 1.49 -- 82.00 73.00 179.25 50
 31 \w 50.00 76.00 1.00 1.49 -- 82.00 73.00 179.25 26
 32 \w 58.00 96.00 1.00 1.49 -- 86.00 63.00 5.27 38
 33 \w 57.00 83.00 1.00 1.49 -- 86.00 65.00 -93.29 26
 34 \w 55.00 82.00 1.00 1.49 -- 86.00 72.00-136.82 27
 35 \w 57.00 82.00 1.00 1.49 -- 86.00 67.00-109.41 25
 36 \w 16.00 108.00 1.00 1.49 -- 94.00-102.00 120.28 92
 37 \w 131.00 169.00 1.00 1.49 -- 104.49 125.00 -90.00 38
 38 \w 143.00 172.00 1.00 1.49 -- 104.49 61.00 -30.00 29
 39 \w 75.00 154.00 1.00 1.49 -- 104.49 61.00 30.00 79
 40 \w 75.00 140.00 1.00 1.49 -- 104.49 61.00 -30.00 65
 41 \w 81.00 175.00 1.00 1.49 -- 104.49 61.00 -90.00 94
 42 \w 120.00 170.00 1.00 1.49 -- 104.49 125.00 -30.00 50
 43 \w 23.00 103.00 1.00 1.49 -- 104.49 -94.00 0.00 80
 44 \w 76.00 133.00 1.00 1.49 -- 104.49 61.00-120.00 57
 45 \w 24.00 88.00 1.00 1.49 -- 104.49 -94.00 -90.00 64
 46 \w 61.00 113.00 1.00 1.49 -- 104.49-125.00-120.00 52
 47 \w 120.00 176.00 1.00 1.49 -- 104.49 61.00 -60.00 56
 48 \w 75.00 101.00 1.00 1.49 -- 104.49 61.00 -60.00 26
 49 \w 116.00 155.00 1.00 1.49 -- 104.49 61.00-180.00 39
 50 \w 75.00 102.00 1.00 1.49 -- 104.49 61.00-180.00 27
 51 \w 121.00 148.00 1.00 1.49 -- 104.49 61.00 120.00 27
 52 \w 75.00 101.00 1.00 1.49 -- 104.49 61.00 90.00 26
 53 \w 111.00 163.00 1.00 1.49 -- 104.49 61.00 90.00 52
 54 \w 75.00 173.00 1.00 1.49 -- 104.49 61.00 150.00 98
 55 \w 75.00 102.00 1.00 1.49 -- 104.49 61.00 120.00 27
 56 \w 27.00 97.00 1.00 1.49 -- 104.49 -94.00 60.00 70
 57 \w 75.00 177.00 1.00 1.49 -- 104.49 61.00 60.00 102
 58 \w 111.00 176.00 1.00 1.49 -- 104.49 61.00 0.00 65
 59 \w 79.00 106.00 1.00 1.49 -- 104.49 61.00 0.00 27
 60 \w 125.00 176.00 1.00 1.49 -- 104.49 61.00-150.00 51
 61 \w 42.00 113.00 1.00 1.49 -- 104.49-125.00 0.00 71
 62 \w 77.00 104.00 1.00 1.49 -- 104.49 61.00-150.00 27
;
_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      0.0183385000
_diffrn_orient_matrix_UB_12      -0.0268345000
_diffrn_orient_matrix_UB_13      -0.0842392000
_diffrn_orient_matrix_UB_21      0.0000752000
_diffrn_orient_matrix_UB_22      0.0676473000
_diffrn_orient_matrix_UB_23      -0.0356619000
_diffrn_orient_matrix_UB_31      0.0707446000
_diffrn_orient_matrix_UB_32      0.0069121000
_diffrn_orient_matrix_UB_33      0.0218626000
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            65063
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.804
_diffrn_reflns_theta_min         3.417
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58608
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       plate
_exptl_crystal_F_000             2624
_exptl_crystal_preparation
'Acid-base reaction between an amine-stabilised alane and the aminoenoate'
_exptl_crystal_recrystallization_method
'Grown from a saturated solution in hexane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 3255 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7178
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+2.3418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                6974
_reflns_number_total             7178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03365d2.cif
_cod_data_source_block           xstr1336
_cod_depositor_comments
'Adding full bibliography for 7708993--7708999.cif.'
_cod_original_cell_volume        7276.35(8)
_cod_database_code               7708998
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C256 H376 Al8 N24 O32 '
_chemical_oxdiff_usercomment     'CEK KLM'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C17 \\sim C16 \\sim C18: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
3. Others
 Fixed Sof: H23A(0.6) H23B(0.6) H23C(0.4) H23D(0.4) C24(0.6) H24A(0.6)
 H24B(0.6) H24C(0.6) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C36A(0.5) H36D(0.5)
 H36E(0.5) H36F(0.5) C24A(0.4) H24D(0.4) H24E(0.4) H24F(0.4)
4.a Ternary CH refined with riding coordinates:
 C32(H32), C13(H13), C35(H35), C16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C23(H23A,H23B), C23(H23C,H23D)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C21(H21), C10(H10), C29(H29), C27(H27), C28(H28), C11(H11)
4.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C15(H15A,H15B,H15C), C34(H34A,H34B,H34C), C1(H1A,H1B,
 H1C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C33(H33A,H33B,H33C), C37(H37A,H37B,
 H37C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C36(H36A,H36B,H36C), C18(H18A,
 H18B,H18C), C36A(H36D,H36E,H36F), C24A(H24D,H24E,H24F)
;
_shelx_res_checksum              43021
_olex2_date_sample_data_collection 2021-04-01
_olex2_exptl_crystal_mounting_method 'On a nylon wire loop under a flow of N2'
_olex2_submission_original_sample_id AlH(AMEDip)2
_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 2.084
_oxdiff_exptl_absorpt_empirical_full_min 0.716