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_7708997
_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 Cl Ga N2 O4'
_chemical_formula_sum            'C36 H52 Cl Ga N2 O4'
_chemical_formula_weight         681.96
_chemical_name_systematic
'Gallium chlorido bis-2,6-diisopropylamidoenoate'
_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                 96.4410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.97530(10)
_cell_length_b                   23.7494(2)
_cell_length_c                   16.86750(10)
_cell_measurement_reflns_used    43130
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.5140
_cell_measurement_theta_min      4.5140
_cell_volume                     3572.75(5)
_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(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 0.998
_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    -91.00 -15.00   1.00    1.00    --  -42.75 -57.00  60.00   76
  2  \w   -113.00 -15.00   1.00    1.00    --  -42.75 -57.00 -30.00   98
  3  \w   -115.00 -17.00   1.00    1.00    --  -42.75 -57.00 150.00   98
  4  \w    -68.00  -6.00   1.00    1.00    --  -42.75 125.00  30.00   62
  5  \w   -108.00 -15.00   1.00    1.00    --  -42.75 -57.00-150.00   93
  6  \w   -115.00 -62.00   1.00    1.00    --  -42.75-152.00 150.00   53
  7  \w    -82.00  -6.00   1.00    1.00    --  -42.75 125.00 120.00   76
  8  \w     10.00  40.00   1.00    1.00    --   42.75  78.00-178.19   30
  9  \w      6.00  64.00   1.00    1.00    --   42.75 -99.00   0.00   58
 10  \w     10.00  39.00   1.00    1.00    --   42.75  77.00 100.14   29
 11  \w     15.00  41.00   1.00    1.00    --   42.75  71.00  39.50   26
 12  \w     79.00 107.00   1.00    1.00    --   42.75  72.00 -91.56   28
 13  \w     14.00  53.00   1.00    1.00    --   42.75  73.00 -26.79   39
 14  \w     13.00  69.00   1.00    1.00    --   42.75  72.00 -91.56   56
 15  \w     89.00 117.00   1.00    1.00    --   42.75  73.00 -26.79   28
 16  \w     70.00 108.00   1.00    1.00    --   42.75  71.00  39.50   38
 17  \w     74.00 177.00   1.00    1.00    --  104.49  66.00  81.07  103
 18  \w     76.00 103.00   1.00    1.00    --  104.49  57.00-160.78   27
 19  \w     75.00 103.00   1.00    1.00    --  104.49  65.00-117.91   28
 20  \w     74.00 129.00   1.00    1.00    --  104.49  70.00 -57.77   55
 21  \w     75.00 102.00   1.00    1.00    --  104.49  65.00 -15.91   27
 22  \w     74.00 175.00   1.00    1.00    --  104.49  70.00 -83.86  101
 23  \w    127.00 177.00   1.00    1.00    --  104.49  63.00 104.81   50
 24  \w     75.00 106.00   1.00    1.00    --  104.49 -94.00  90.00   31
 25  \w     74.00 178.00   1.00    1.00    --  104.49  69.00-137.49  104
 26  \w     24.00 101.00   1.00    1.00    --  104.49 -94.00 -60.00   77
 27  \w    108.00 178.00   1.00    1.00    --  104.49  67.00 159.76   70
 28  \w     35.00 105.00   1.00    1.00    --  104.49 -94.00-180.00   70
 29  \w     31.00 106.00   1.00    1.00    --  104.49 -94.00   0.00   75
 30  \w     74.00 101.00   1.00    1.00    --  104.49  67.00 159.76   27
 31  \w     75.00 101.00   1.00    1.00    --  104.49  63.00 104.81   26
 32  \w     74.00 149.00   1.00    1.00    --  104.49  67.00  16.21   75
 33  \w     75.00 101.00   1.00    1.00    --  104.49  61.00   0.00   26
 34  \w     75.00 119.00   1.00    1.00    --  104.49  64.00  33.86   44
 35  \w    143.00 170.00   1.00    1.00    --  104.49  74.00  -7.83   27
 36  \w     75.00 102.00   1.00    1.00    --  104.49  61.00 120.00   27
 37  \w    124.00 162.00   1.00    1.00    --  104.49  58.00  55.98   38
 38  \w     33.00 132.00   1.00    1.00    --  104.49 -61.00  30.00   99
 39  \w     75.00 135.00   1.00    1.00    --  104.49  61.00 150.00   60
 40  \w     76.00 120.00   1.00    1.00    --  104.49  58.00  55.98   44
 41  \w     75.00 145.00   1.00    1.00    --  104.49  61.00-150.00   70
 42  \w     75.00 101.00   1.00    1.00    --  104.49  61.00 -60.00   26
 43  \w     75.00 102.00   1.00    1.00    --  104.49  61.00 -30.00   27
 44  \w     73.00 100.00   1.00    1.00    --  104.49  74.00  -7.83   27
 45  \w     76.00 102.00   1.00    1.00    --  104.49  59.00  72.76   26
 46  \w     75.00 102.00   1.00    1.00    --  104.49  61.00-180.00   27
 47  \w    123.00 164.00   1.00    1.00    --  104.49  61.00 -90.00   41
 48  \w     75.00 117.00   1.00    1.00    --  104.49  61.00 -90.00   42
 49  \w    109.00 178.00   1.00    1.00    --  104.49  72.00 -36.99   69
 50  \w     75.00 102.00   1.00    1.00    --  104.49  61.00  60.00   27
 51  \w     97.00 178.00   1.00    1.00    --  104.49 125.00   0.00   81
 52  \w     73.00 101.00   1.00    1.00    --  104.49  72.00 -36.99   28
 53  \w     76.00 112.00   1.00    1.00    --  104.49  58.00 138.49   36
;
_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  0.0454
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            60788
_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         72.689
_diffrn_reflns_theta_min         4.563
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.045
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59215
_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    1.268
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_preparation
'Reaction of gallium chloride with lithium salt of ligand in hexane'
_exptl_crystal_recrystallization_method
'crystallised from a solution of hexane'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+1.5400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6734
_reflns_number_total             7039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03365d2.cif
_cod_data_source_block           xstr1131
_cod_depositor_comments
'Adding full bibliography for 7708993--7708999.cif.'
_cod_database_code               7708997
_shelx_shelxl_version_number     2018/3
_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. Others
 Fixed Sof: H5AA(0.4) H5AB(0.4) H5BC(0.6) H5BD(0.6) C6(0.4) H6A(0.4) H6B(0.4)
 H6C(0.4) C6A(0.6) H6AA(0.6) H6AB(0.6) H6AC(0.6)
3.a Ternary CH refined with riding coordinates:
 C31(H31), C13(H13), C34(H34), C16(H16)
3.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C5(H5AA,H5AB), C5(H5BC,H5BD)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C21(H21), C9(H9), C27(H27), C10(H10), C11(H11), C29(H29), C28(H28)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C36(H36A,H36B,H36C), C33(H33A,H33B,
 H33C), C14(H14A,H14B,H14C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C17(H17A,
 H17B,H17C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C),
 C6(H6A,H6B,H6C), C6A(H6AA,H6AB,H6AC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              735
_shelx_fab_checksum              67108
_olex2_exptl_crystal_mounting_method
'Crystal mounted on a nylon loop after being submerged in frombin oil.'
_olex2_submission_original_sample_id GaClAMEDip2
_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
;