Lithium diamidodihydridoaluminates: bimetallic cooperativity in catalytic hydroboration and metallation applications
Pollard, Victoria A.; Orr, Samantha A.; McLellan, Ross; Kennedy, Alan R.; Hevia, Eva; Mulvey, Robert E.; Chemical Communications  (2018) –; doi:10.1039/C7CC08214B

data_7121151
_publ_section_title
;
 Lithium diamidodihydridoaluminates: bimetallic cooperativity in catalytic
 hydroboration and metallation applications
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C7CC08214B
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C20 H54 Al Li N2 O4 Si4, C7 H8'
_chemical_formula_sum            'C27 H62 Al Li N2 O4 Si4'
_chemical_formula_weight         625.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-10-10
_audit_creation_method
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
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_audit_update_record
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2017-10-12 deposited with the CCDC.
2017-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3904(3)
_cell_length_b                   14.4124(3)
_cell_length_c                   21.2850(5)
_cell_measurement_reflns_used    15751
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      72.9640
_cell_measurement_theta_min      5.1580
_cell_volume                     3800.98(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_detector                 'CCD plate'
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_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.9862
_diffrn_measured_fraction_theta_max 0.9855
_diffrn_measurement_details
;
  1 omega  -69.00   21.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 90

  2 omega  -21.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 90

  3 omega  -13.00   77.00   1.0000   18.6150
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000   30.0000 90

  4 omega   35.00  125.00   1.0000   18.6150
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000 -180.0000 90

  5 omega  -16.00   82.00   1.0000   18.6150
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -37.0000  -90.0000 98

  6 omega  -17.00  100.00   1.0000   18.6150
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -19.0000 -180.0000 117

  7 omega  -14.00   86.00   1.0000   18.6150
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -77.0000  150.0000 100

  8 omega   18.00  113.00   1.0000   18.6150
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000  -60.0000 95

  9 omega   42.00  142.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   90.0000 100

 10 omega   40.00  116.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -180.0000 76

 11 omega  100.00  178.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000 -150.0000 78

 12 omega   42.00  142.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  -90.0000 100

 13 omega   78.00  178.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000   30.0000 100

 14 omega   40.00  116.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -90.0000 76

 15 omega   40.00   92.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000 -180.0000 52

 16 omega   40.00   92.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000  -90.0000 52

 17 omega   39.00   94.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000  120.0000 55

 18 omega   78.00  178.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000  150.0000 100

 19 omega   40.00   90.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000  -30.0000 50

 20 omega   42.00  122.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -126.0000  119.0000 80

 21 omega   42.00   91.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -150.0000 49

 22 omega   41.00   92.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000   30.0000 51

 23 omega   40.00   92.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000   90.0000 52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0465721000
_diffrn_orient_matrix_UB_12      0.0001330000
_diffrn_orient_matrix_UB_13      0.0670589000
_diffrn_orient_matrix_UB_21      -0.1135858000
_diffrn_orient_matrix_UB_22      -0.0178218000
_diffrn_orient_matrix_UB_23      -0.0266789000
_diffrn_orient_matrix_UB_31      0.0191836000
_diffrn_orient_matrix_UB_32      -0.1054482000
_diffrn_orient_matrix_UB_33      0.0045957000
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30698
_diffrn_reflns_theta_full        73.4853
_diffrn_reflns_theta_max         73.49
_diffrn_reflns_theta_min         3.70
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.908
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.0922
_exptl_crystal_description       needle
_exptl_crystal_F_000             1375.9205
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.2883
_refine_diff_density_min         -0.2592
_refine_diff_density_rms         0.0475
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.044(16)
_refine_ls_d_res_high            0.8041
_refine_ls_d_res_low             11.9340
_refine_ls_goodness_of_fit_ref   1.0222
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    86
_refine_ls_number_parameters     373
_refine_ls_number_reflns         7551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0222
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0595P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                7190
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_cod_data_source_file            c7cc08214b2.cif
_cod_data_source_block           VP1704
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7121151
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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 Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C14(H14a,H14b), C15(H15a,H15b), C16(H16a,H16b), C17(H17a,
 H17b), C18(H18a,H18b), C19(H19a,H19b), C20(H20a,H20b)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C5(H5a,
 H5b,H5c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c),
 C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C21(H21a,H21b,
 H21c)
;
_olex2_submission_special_instructions 'No special instructions were received'