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_7121150
_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         'C28 H70 Al N2 Na O4 Si4'
_chemical_formula_sum            'C28 H70 Al N2 Na O4 Si4'
_chemical_formula_weight         661.19
_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             2017-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8589(2)
_cell_length_b                   16.0231(2)
_cell_length_c                   19.8745(4)
_cell_measurement_reflns_used    20065
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      72.9220
_cell_measurement_theta_min      4.4190
_cell_volume                     4094.93(12)
_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 0.9872
_diffrn_measured_fraction_theta_max 0.9872
_diffrn_measurement_details
;
  1 omega  -21.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 90

  2 omega  -69.00   21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 90

  3 omega   26.00  126.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  -60.0000 100

  4 omega   18.00  113.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000  120.0000 95

  5 omega   26.00  126.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  150.0000 100

  6 omega  -13.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000  -60.0000 90

  7 omega   30.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   37.0000   90.0000 98

  8 omega  -13.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000 -180.0000 90

  9 omega   90.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   63.0000  120.0000 88

 10 omega   42.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  -90.0000 63

 11 omega   78.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000 -150.0000 100

 12 omega   39.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000    0.0000 55

 13 omega   39.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -150.0000 55

 14 omega   42.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -150.0000 63

 15 omega   90.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000 -120.0000 88

 16 omega   39.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000  -60.0000 55

 17 omega   39.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000   60.0000 55

 18 omega   40.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -180.0000 76

 19 omega   42.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  120.0000 63

 20 omega   40.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   60.0000 76

 21 omega   40.00  150.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -91.0000 -120.0000 110

 22 omega   44.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -63.0000   30.0000 90

 23 omega  -21.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   90.0000 90

 24 omega   -4.00   42.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   60.0000 46

 25 omega   35.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000 -120.0000 64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0431032000
_diffrn_orient_matrix_UB_12      -0.0234798000
_diffrn_orient_matrix_UB_13      -0.0697902000
_diffrn_orient_matrix_UB_21      -0.0549740000
_diffrn_orient_matrix_UB_22      0.0762793000
_diffrn_orient_matrix_UB_23      -0.0309289000
_diffrn_orient_matrix_UB_31      0.0974118000
_diffrn_orient_matrix_UB_32      0.0535192000
_diffrn_orient_matrix_UB_33      0.0134566000
_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  0.0259
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33288
_diffrn_reflns_theta_full        73.3610
_diffrn_reflns_theta_max         73.36
_diffrn_reflns_theta_min         3.54
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.891
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46503
_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    1.0724
_exptl_crystal_description       block
_exptl_crystal_F_000             1464.5131
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.5011
_refine_diff_density_min         -0.2252
_refine_diff_density_rms         0.0532
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.003(16)
_refine_ls_d_res_high            0.8046
_refine_ls_d_res_low             12.4740
_refine_ls_goodness_of_fit_ref   1.0812
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    109
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8122
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.0749
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.8754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.980
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              24
_reflns_limit_l_min              -24
_reflns_number_gt                7995
_reflns_number_total             8122
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7cc08214b2.cif
_cod_data_source_block           VP1705
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7121150
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C25-C26 = C26-C27 = C27-C28
 1.53 with sigma of 0.01
 C25A-C26A = C26A-C27A = C27A-C28A
 1.53 with sigma of 0.01
 O4-C28 = O4-C25 = O4-C28A = O4-C25A
 1.43 with sigma of 0.01
3. Rigid bond restraints
 O4, C28A, C26A, C25A, C27A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O4 \\sim C28A \\sim C26A \\sim C25A \\sim C27A: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
O4 \\sim C25 \\sim C26 \\sim C27 \\sim C28: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
5. Others
 Sof(C28A)=Sof(H28c)=Sof(H28d)=Sof(C26A)=Sof(H26c)=Sof(H26d)=Sof(C25A)=
 Sof(H25c)=Sof(H25d)=Sof(C27A)=Sof(H27c)=Sof(H27d)=1-FVAR(1)
 Sof(C25)=Sof(H25a)=Sof(H25b)=Sof(C26)=Sof(H26a)=Sof(H26b)=Sof(C27)=Sof(H27a)=
 Sof(H27b)=Sof(C28)=Sof(H28a)=Sof(H28b)=FVAR(1)
6.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), C21(H21a,H21b),
 C22(H22a,H22b), C23(H23a,H23b), C24(H24a,H24b), C25(H25a,H25b), C26(H26a,H26b),
  C27(H27a,H27b), C28(H28a,H28b), C28A(H28c,H28d), C26A(H26c,H26d), C25A(H25c,
 H25d), C27A(H27c,H27d)
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)
;
_olex2_submission_special_instructions 'No special instructions were received'