Diverse outcomes of CO2 fixation using alkali metal amides including formation of a heterobimetallic lithium–sodium carbamato-anhydride via lithium–sodium bis-hexamethyldisilazide
Gauld, Richard M.; Kennedy, Alan R.; McLellan, Ross; Barker, Jim; Reid, Jacqueline; Mulvey, Robert E.; Chemical Communications  (2019) –; doi:10.1039/C8CC08308H

data_7122842
_publ_section_title
;
 Diverse outcomes of CO2 fixation using alkali metal amides including
 formation of a heterobimetallic lithium--sodium carbamato-anhydride via
 lithium--sodium bis-hexamethyldisilazide
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08308H
_journal_year                    2019
_chemical_formula_moiety         'C98 H198 Li12 N14 O28'
_chemical_formula_sum            'C98 H198 Li12 N14 O28'
_chemical_formula_weight         2104.02
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-06-04
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Olex2 1.2
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2018-10-12 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                110.729(4)
_cell_angle_beta                 95.790(3)
_cell_angle_gamma                98.130(4)
_cell_formula_units_Z            1
_cell_length_a                   14.8500(7)
_cell_length_b                   15.5422(6)
_cell_length_c                   17.5104(7)
_cell_measurement_reflns_used    10007
_cell_measurement_temperature    153(2)
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
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CrysAlisPro, Agilent Technologies,
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omega____ theta____ kappa____ phi______ frames
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omega____ theta____ kappa____ phi______ frames
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omega____ theta____ kappa____ phi______ frames
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  5 omega  -17.00  100.00   1.0000    6.2150
omega____ theta____ kappa____ phi______ frames
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  6 omega  -13.00   77.00   1.0000    6.2150
omega____ theta____ kappa____ phi______ frames
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  7 omega  -14.00   86.00   1.0000    6.2150
omega____ theta____ kappa____ phi______ frames
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  8 omega   39.00   94.00   1.0000    6.2150
omega____ theta____ kappa____ phi______ frames
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  9 omega   40.00  150.00   1.0000    6.2150
omega____ theta____ kappa____ phi______ frames
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 10 omega   44.00  134.00   1.0000    6.2150
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 11 omega   86.00  178.00   1.0000    6.2150
omega____ theta____ kappa____ phi______ frames
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 12 omega   56.00  150.00   1.0000    6.2150
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 13 omega   40.00  116.00   1.0000    6.2150
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 15 omega  100.00  178.00   1.0000    6.2150
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -60.0000 78

 16 omega   90.00  178.00   1.0000    6.2150
omega____ theta____ kappa____ phi______ frames
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 17 omega   42.00  105.00   1.0000    6.2150
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 18 omega   40.00  116.00   1.0000    6.2150
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 19 omega   39.00   94.00   1.0000    6.2150
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 20 omega   90.00  178.00   1.0000    6.2150
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omega____ theta____ kappa____ phi______ frames
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omega____ theta____ kappa____ phi______ frames
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 23 omega  -73.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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omega____ theta____ kappa____ phi______ frames
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 26 omega   35.00  125.00   1.0000    6.2150
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000   30.0000 90
;
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_diffrn_orient_matrix_UB_31      -0.0572433000
_diffrn_orient_matrix_UB_32      -0.0991824000
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_diffrn_radiation_monochromator  graphite
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_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.540
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_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)
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Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            colourless
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'w=1/[\s^2^(Fo^2^)+(0.1892P)^2^+0.7468P] where P=(Fo^2^+2Fc^2^)/3'
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_olex2_refinement_description
;
PLATON SQUEEZE used to remove traces of disordered solvent.

Approx 102 electorn equivalents were removed from 818 cubic
A of cell volume.

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C3-C4 = C3-C5 = C3A-C4A = C3A-C5A = C30-C32 = C30-C33
 1.53 with sigma of 0.01
 C17-C18 = C17-C19 = C17A-C18A = C17A-C19A
 1.53 with sigma of 0.01
 C31-C34 = C31-C35 = C31A-C34A = C31A-C35A = C30A-C32A = C30A-C33A
 1.53 with sigma of 0.01
 C3-N1 = C3A-N1 = N5-C30 = N5-C31 = N5-C30A = N5-C31A = N3-C17
 1.47 with sigma of 0.01
 N3-C17A
 1.47 with sigma of 0.01
3. Rigid bond restraints
 N1, C3, C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, C30, C31, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C3 \\sim C4 \\sim C5: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.02
N5 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.02
N3 \\sim C17 \\sim C18 \\sim C19: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C3) = Uanis(C3A)
Uanis(C4) = Uanis(C4A)
Uanis(C5) = Uanis(C5A)
Uanis(C17) = Uanis(C17A)
Uanis(C18) = Uanis(C18A)
Uanis(C19) = Uanis(C19A)
Uanis(C30) = Uanis(C30A)
Uanis(C31) = Uanis(C31A)
Uanis(C32) = Uanis(C32A)
Uanis(C33) = Uanis(C33A)
Uanis(C34) = Uanis(C34A)
Uanis(C35) = Uanis(C35A)
5. Others
 Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=Sof(H4Ac)=Sof(C5A)=Sof(H5Aa)=
 Sof(H5Ab)=Sof(H5Ac)=1-FVAR(1)
 Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4a)=Sof(H4b)=Sof(H4c)=Sof(C5)=Sof(H5a)=Sof(H5b)=
 Sof(H5c)=FVAR(1)
 Sof(C31A)=Sof(H31A)=Sof(C30A)=Sof(H30A)=Sof(C32A)=Sof(H32d)=Sof(H32e)=
 Sof(H32f)=Sof(C33A)=Sof(H33d)=Sof(H33e)=Sof(H33f)=Sof(C34A)=Sof(H34d)=
 Sof(H34e)=Sof(H34f)=Sof(C35A)=Sof(H35d)=Sof(H35e)=Sof(H35f)=1-FVAR(2)
 Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32a)=Sof(H32b)=Sof(H32c)=
 Sof(C33)=Sof(H33a)=Sof(H33b)=Sof(H33c)=Sof(C34)=Sof(H34a)=Sof(H34b)=Sof(H34c)=
 Sof(C35)=Sof(H35a)=Sof(H35b)=Sof(H35c)=FVAR(2)
 Sof(C17A)=Sof(H17A)=Sof(C19A)=Sof(H19d)=Sof(H19e)=Sof(H19f)=Sof(C18A)=
 Sof(H18d)=Sof(H18e)=Sof(H18f)=1-FVAR(3)
 Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18a)=Sof(H18b)=Sof(H18c)=Sof(C19)=Sof(H19a)=
 Sof(H19b)=Sof(H19c)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C9(H9), C10(H10), C16(H16), C17(H17), C23(H23), C24(H24),
 C30(H30), C31(H31), C37(H37), C38(H38), C44(H44), C45(H45), C3A(H3A),
 C31A(H31A), C30A(H30A), C17A(H17A)
6.b Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C11(H11a,
 H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C14(H14a,H14b,H14c),
 C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C21(H21a,H21b,
 H21c), C25(H25a,H25b,H25c), C26(H26a,H26b,H26c), C27(H27a,H27b,H27c), C28(H28a,
 H28b,H28c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C34(H34a,H34b,H34c),
 C35(H35a,H35b,H35c), C39(H39a,H39b,H39c), C40(H40a,H40b,H40c), C41(H41a,H41b,
 H41c), C42(H42a,H42b,H42c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,
 H48b,H48c), C49(H49a,H49b,H49c), C4A(H4Aa,H4Ab,H4Ac), C5A(H5Aa,H5Ab,H5Ac),
 C32A(H32d,H32e,H32f), C33A(H33d,H33e,H33f), C34A(H34d,H34e,H34f), C35A(H35d,
 H35e,H35f), C19A(H19d,H19e,H19f), C18A(H18d,H18e,H18f)
6.c Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'