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_7121153
_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_formula_moiety         'C21 H61 Al Li N5 Si4'
_chemical_formula_sum            'C21 H61 Al Li N5 Si4'
_chemical_formula_weight         530.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-04-01
_audit_creation_method
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Olex2 1.2
(compiled Mar  2 2017 14:02:25 for OlexSys, GUI svn.r5324)
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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                 93.426(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2497(3)
_cell_length_b                   11.7867(2)
_cell_length_c                   16.1366(3)
_cell_measurement_reflns_used    16238
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      73.1090
_cell_measurement_theta_min      4.4350
_cell_volume                     3464.84(10)
_computing_cell_refinement
;
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_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)
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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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;
  1 omega   -4.00   42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   60.0000 46

  2 omega  -30.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -180.0000 100

  3 omega  -14.00   86.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -77.0000 -180.0000 100

  4 omega   30.00  128.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   37.0000 -180.0000 98

  5 omega   -4.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -99.0000  -30.0000 102

  6 omega   35.00  125.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000   30.0000 90

  7 omega   35.00  125.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000  -90.0000 90

  8 omega  -13.00   77.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000   60.0000 90

  9 omega   90.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   63.0000 -120.0000 88

 10 omega   39.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -150.0000 55

 11 omega   40.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -30.0000 76

 12 omega   42.00  142.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  -30.0000 100

 13 omega   56.00  150.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  179.0000  150.0000 94

 14 omega   40.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -120.0000 76

 15 omega   40.00   92.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000  150.0000 52

 16 omega   40.00   92.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000  -60.0000 52

 17 omega   40.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  150.0000 76

 18 omega   40.00   92.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000  -90.0000 52

 19 omega   40.00   92.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000   99.0000 52

 20 omega   42.00  105.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000   90.0000 63

 21 omega   39.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000    0.0000   30.0000 139

 22 omega   42.00  142.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  150.0000 100

 23 omega  -69.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 90

 24 omega  -72.00   26.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -37.0000   90.0000 98

 25 omega   35.00  125.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000   90.0000 90

 26 omega   26.00  112.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  -60.0000 86

 27 omega   35.00  125.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000 -150.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0403746000
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_diffrn_orient_matrix_UB_31      -0.0742877000
_diffrn_orient_matrix_UB_32      0.0582678000
_diffrn_orient_matrix_UB_33      0.0113523000
_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  0.0567
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31783
_diffrn_reflns_theta_full        70.0000
_diffrn_reflns_theta_max         73.12
_diffrn_reflns_theta_min         4.47
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.951
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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)
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    1.0160
_exptl_crystal_description       block
_exptl_crystal_F_000             1182.9765
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.4023
_refine_diff_density_min         -0.2559
_refine_diff_density_rms         0.0614
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_refine_ls_d_res_low             9.8960
_refine_ls_goodness_of_fit_ref   1.0459
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    80
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0459
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.0016
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+1.1279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1040
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_reflns_limit_h_min              -22
_reflns_limit_k_max              14
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_reflns_limit_l_min              0
_reflns_number_gt                6189
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_cod_data_source_file            c7cc08214b2.cif
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_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C4(H4a,H4b), C6(H6a,H6b), C7(H7a,H7b)
2.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C2(H2a,H2b,H2c), C5(H5a,H5b,H5c), C8(H8a,H8b,H8c), C9(H9a,
 H9b,H9c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c),
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,
 H16c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C20(H20a,
 H20b,H20c), C21(H21a,H21b,H21c)
;
_olex2_submission_special_instructions 'No special instructions were received'