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_7121149
_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         'C13 H32 Al Li N4 O Si2'
_chemical_formula_sum            'C13 H32 Al Li N4 O Si2'
_chemical_formula_weight         350.52
_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     direct
_audit_creation_date             2016-12-13
_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                 96.332(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3714(7)
_cell_length_b                   14.1997(7)
_cell_length_c                   11.4816(7)
_cell_measurement_reflns_used    2937
_cell_measurement_temperature    160.3
_cell_measurement_theta_max      27.4968
_cell_measurement_theta_min      2.8632
_cell_volume                     2166.7(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
;
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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      160.3
_diffrn_detector_area_resol_mean 16.0727
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
  1 omega  -83.00    1.00   1.0000  152.1800
omega____ theta____ kappa____ phi______ frames
    -      -18.0350  -21.0000 -122.0000 84

  2 omega  -80.00   19.00   1.0000  152.1800
omega____ theta____ kappa____ phi______ frames
    -      -18.0350  -21.0000  -44.0000 99

  3 omega  -94.00  -64.00   1.0000  152.1800
omega____ theta____ kappa____ phi______ frames
    -      -18.0350  163.0000  -79.0000 30

  4 omega  -90.00  -65.00   1.0000  152.1800
omega____ theta____ kappa____ phi______ frames
    -      -18.0350  -37.0000  150.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0415905000
_diffrn_orient_matrix_UB_12      -0.0109787000
_diffrn_orient_matrix_UB_13      -0.0308709000
_diffrn_orient_matrix_UB_21      0.0298902000
_diffrn_orient_matrix_UB_22      -0.0085757000
_diffrn_orient_matrix_UB_23      0.0539709000
_diffrn_orient_matrix_UB_31      -0.0148591000
_diffrn_orient_matrix_UB_32      -0.0479540000
_diffrn_orient_matrix_UB_33      -0.0025491000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10020
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.869
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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    1.075
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4611
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+1.9218P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.2310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2713
_reflns_number_total             4611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08214b2.cif
_cod_data_source_block           RMSO20
_cod_database_code               7121149
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.00
_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
 O1A-C13A
 1.43 with sigma of 0.02
 O1A-C10A
 1.43 with sigma of 0.02
 O1-C13 = O1-C10
 1.43 with sigma of 0.02
 C12-C13 = C11-C12 = C10-C11
 1.54 with sigma of 0.02
 C11A-C10A = C12A-C11A = C13A-C12A
 1.54 with sigma of 0.02
3. Rigid bond restraints
 O1, C10, C13, C12, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim C10 \\sim C13 \\sim C12 \\sim C11: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(O1) = Uanis(O1A)
Uanis(C10) = Uanis(C10A)
Uanis(C11) = Uanis(C11A)
Uanis(C12) = Uanis(C12A)
Uanis(C13) = Uanis(C13A)
5. Others
 Sof(O1A)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(C13A)=Sof(H13A)=Sof(H13B)=
 Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=1-FVAR(1)
 Sof(O1)=Sof(C10)=Sof(H10C)=Sof(H10D)=Sof(C13)=Sof(H13C)=Sof(H13D)=Sof(C12)=
 Sof(H12C)=Sof(H12D)=Sof(C11)=Sof(H11C)=Sof(H11D)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C10A(H10A,H10B), C13A(H13A,H13B), C11A(H11A,H11B), C12A(H12A,H12B), C10(H10C,
 H10D), C13(H13C,H13D), C12(H12C,H12D), C11(H11C,H11D)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_olex2_submission_original_sample_id RMSO20
_olex2_submission_special_instructions 'No special instructions were received'