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_7121152
_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         'C12 H38 Al N2 Si4, C12 H32 Li N4'
_chemical_formula_sum            'C24 H70 Al Li N6 Si4'
_chemical_formula_weight         589.13
_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             2017-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-12 deposited with the CCDC.
2017-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.296(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8785(3)
_cell_length_b                   12.5619(2)
_cell_length_c                   17.5361(3)
_cell_measurement_reflns_used    15022
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      73.1380
_cell_measurement_theta_min      4.2940
_cell_volume                     3938.34(11)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0268
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.9905
_diffrn_measured_fraction_theta_max 0.9880
_diffrn_measurement_details
;
  1 omega  -30.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   60.0000 100

  2 omega   -4.00   42.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -90.0000 46

  3 omega   26.00  126.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  -30.0000 100

  4 omega   18.00  113.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000 -120.0000 95

  5 omega   26.00  126.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000    0.0000 100

  6 omega   -4.00   98.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -99.0000  150.0000 102

  7 omega   26.00  126.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000   60.0000 100

  8 omega   26.00  126.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  -90.0000 100

  9 omega   40.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000   60.0000 52

 10 omega   42.00  105.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  -30.0000 63

 11 omega   44.00  134.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -63.0000   90.0000 90

 12 omega   40.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000 -120.0000 52

 13 omega   41.00  126.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -134.0000 -112.0000 85

 14 omega   90.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000 -180.0000 88

 15 omega   42.00  105.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  -60.0000 63

 16 omega   39.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000    0.0000 55

 17 omega   40.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -90.0000 76

 18 omega   86.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   37.0000    0.0000 92

 19 omega   40.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  120.0000 76

 20 omega   42.00  105.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -180.0000 63

 21 omega   39.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -12.0000  150.0000 139

 22 omega   40.00  150.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -91.0000  -60.0000 110

 23 omega  -21.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 90

 24 omega  -44.00   73.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000  -90.0000 117

 25 omega   26.00  126.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000 -180.0000 100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0153040000
_diffrn_orient_matrix_UB_12      0.0989523000
_diffrn_orient_matrix_UB_13      0.0495266000
_diffrn_orient_matrix_UB_21      -0.0848120000
_diffrn_orient_matrix_UB_22      0.0183339000
_diffrn_orient_matrix_UB_23      0.0080954000
_diffrn_orient_matrix_UB_31      -0.0005192000
_diffrn_orient_matrix_UB_32      -0.0701212000
_diffrn_orient_matrix_UB_33      0.0720743000
_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  0.0523
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32432
_diffrn_reflns_theta_full        73.4219
_diffrn_reflns_theta_max         73.42
_diffrn_reflns_theta_min         4.30
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44295
_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    0.9935
_exptl_crystal_description       plate
_exptl_crystal_F_000             1319.3030
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.5338
_refine_diff_density_min         -0.3554
_refine_diff_density_rms         0.0773
_refine_ls_d_res_high            0.8044
_refine_ls_d_res_low             10.2784
_refine_ls_goodness_of_fit_ref   1.0173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    121
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7818
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.0125
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0916P)^2^+1.3147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1458
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -21
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                6487
_reflns_number_total             7818
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7cc08214b2.cif
_cod_data_source_block           VP1703
_cod_database_code               7121152
_chemical_oxdiff_formula         c15h17no5
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_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. Restrained distances
 C21-C22 = C21A-C22A
 1.53 with sigma of 0.01
 N5-C19 = N5-C20 = N5-C21 = N6-C22 = N6-C23 = N6-C24
 1.47 with sigma of 0.01
 N5-C19A = N5-C20A = N5-C21A = N6-C22A = N6-C23A = N6-C24A
 1.47 with sigma of 0.01
3. Rigid bond restraints
 N5, N6, C19, C20, C21, C22, C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N5 \\sim N6 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C19) = Uanis(C19A)
Uanis(C20) = Uanis(C20A)
Uanis(C21) = Uanis(C21A)
Uanis(C22) = Uanis(C22A)
Uanis(C23) = Uanis(C23A)
Uanis(C24) = Uanis(C24A)
5. Others
 Sof(C19A)=Sof(H19d)=Sof(H19e)=Sof(H19f)=Sof(C20A)=Sof(H20d)=Sof(H20e)=
 Sof(H20f)=Sof(C21A)=Sof(H21c)=Sof(H21d)=Sof(C22A)=Sof(H22c)=Sof(H22d)=
 Sof(C23A)=Sof(H23d)=Sof(H23e)=Sof(H23f)=Sof(C24A)=Sof(H24d)=Sof(H24e)=
 Sof(H24f)=1-FVAR(1)
 Sof(C19)=Sof(H19a)=Sof(H19b)=Sof(H19c)=Sof(C20)=Sof(H20a)=Sof(H20b)=Sof(H20c)=
 Sof(C21)=Sof(H21a)=Sof(H21b)=Sof(C22)=Sof(H22a)=Sof(H22b)=Sof(C23)=Sof(H23a)=
 Sof(H23b)=Sof(H23c)=Sof(C24)=Sof(H24a)=Sof(H24b)=Sof(H24c)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15a,H15b), C16(H16a,H16b), C21(H21a,H21b), C22(H22a,H22b), C21A(H21c,
 H21d), C22A(H22c,H22d)
6.b 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), C13(H13a,H13b,
 H13c), C14(H14a,H14b,H14c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C19(H19a,
 H19b,H19c), C20(H20a,H20b,H20c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c),
 C19A(H19d,H19e,H19f), C20A(H20d,H20e,H20f), C23A(H23d,H23e,H23f), C24A(H24d,
 H24e,H24f)
;
_olex2_submission_special_instructions 'No special instructions were received'