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_7121146
_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         'C24 H62 Al Li N2 O3 Si4'
_chemical_formula_sum            'C24 H62 Al Li N2 O3 Si4'
_chemical_formula_weight         573.03
_chemical_name_systematic
;
 ?
;
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
;
_audit_update_record
;
2017-10-12 deposited with the CCDC.
2017-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.154(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1211(7)
_cell_length_b                   11.6571(5)
_cell_length_c                   16.3906(6)
_cell_measurement_reflns_used    10447
_cell_measurement_temperature    151.4
_cell_measurement_theta_max      29.4255
_cell_measurement_theta_min      3.0145
_cell_volume                     3653.4(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_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      151.4
_diffrn_detector_area_resol_mean 16.0727
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega   -6.00   75.00   1.0000   50.0300
omega____ theta____ kappa____ phi______ frames
    -       19.3443 -122.0000   62.0000 81

  2 omega   -6.00   86.00   1.0000   50.0300
omega____ theta____ kappa____ phi______ frames
    -       19.3443   37.0000  -90.0000 92

  3 omega  -53.00   45.00   1.0000   50.0300
omega____ theta____ kappa____ phi______ frames
    -       19.3443  -37.0000   90.0000 98

  4 omega   65.00   93.00   1.0000   50.0300
omega____ theta____ kappa____ phi______ frames
    -       19.3443 -151.0000 -124.0000 28

  5 omega  -87.00   -9.00   1.0000   50.0300
omega____ theta____ kappa____ phi______ frames
    -      -20.1256  142.0000 -125.0000 78

  6 omega  -11.00   89.00   1.0000   50.0300
omega____ theta____ kappa____ phi______ frames
    -       19.3443   77.0000   60.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0081787000
_diffrn_orient_matrix_UB_12      0.0553266000
_diffrn_orient_matrix_UB_13      -0.0152293000
_diffrn_orient_matrix_UB_21      0.0359904000
_diffrn_orient_matrix_UB_22      0.0148280000
_diffrn_orient_matrix_UB_23      0.0008226000
_diffrn_orient_matrix_UB_31      0.0037633000
_diffrn_orient_matrix_UB_32      -0.0204669000
_diffrn_orient_matrix_UB_33      -0.0405061000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36740
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         3.021
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
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    1.042
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         8703
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+1.9900P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1345
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6410
_reflns_number_total             8703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08214b2.cif
_cod_data_source_block           RMSO22
_cod_database_code               7121146
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.01
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.95319 0.04681
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C15-C16 = C15-C14 = C13-C14
 1.53 with sigma of 0.01
 C15A-C16A = C15A-C14A = C13A-C14A
 1.53 with sigma of 0.01
 C23-C24 = C23-C22 = C22-C21
 1.53 with sigma of 0.01
 C23A-C24A = C23A-C22A = C22A-C21A
 1.53 with sigma of 0.01
 C17-C18 = C18-C19 = C19-C20
 1.53 with sigma of 0.01
 C17A-C18A = C18A-C19A = C19A-C20A
 1.53 with sigma of 0.01
 O1-C13 = O1-C16 = O1-C13A = O1-C16A
 1.43 with sigma of 0.01
 O2-C17 = O2-C20 = O2-C17A = O2-C20A
 1.43 with sigma of 0.01
 O3-C21 = O3-C24 = O3-C21A = O3-C24A
 1.43 with sigma of 0.01
4. Rigid bond restraints
 O2, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C21, C22, C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O2 \\sim C17 \\sim C18 \\sim C19 \\sim C20: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.02
O1 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.02
O3 \\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(C13) = Uanis(C13A)
Uanis(C14) = Uanis(C14A)
Uanis(C15) = Uanis(C15A)
Uanis(C16) = Uanis(C16A)
Uanis(C17) = Uanis(C17A)
Uanis(C18) = Uanis(C18A)
Uanis(C19) = Uanis(C19A)
Uanis(C20) = Uanis(C20A)
Uanis(C21) = Uanis(C21A)
Uanis(C22) = Uanis(C22A)
Uanis(C23) = Uanis(C23A)
Uanis(C24) = Uanis(C24A)
6. Others
 Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C15A)=
 Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(H16C)=Sof(H16D)=1-FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=FVAR(1)
 Sof(C17A)=Sof(H17C)=Sof(H17D)=Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=
 Sof(H19C)=Sof(H19D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=1-FVAR(2)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=FVAR(2)
 Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C22A)=
 Sof(H22C)=Sof(H22D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=1-FVAR(3)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=FVAR(3)
7.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), C13A(H13C,H13D), C14A(H14C,
 H14D), C15A(H15C,H15D), C16A(H16C,H16D), C17A(H17C,H17D), C18A(H18C,H18D),
 C19A(H19C,H19D), C20A(H20C,H20D), C21A(H21C,H21D), C23A(H23C,H23D), C22A(H22C,
 H22D), C24A(H24C,H24D)
7.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C2(H2A,
 H2B,H2C), C7(H7A,H7B,H7C), C3(H3A,H3B,H3C), C11(H11A,H11B,H11C), C8(H8A,H8B,
 H8C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C)
;
_olex2_submission_original_sample_id RMSO22
_olex2_submission_special_instructions 'No special instructions were received'