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_7122841
_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         'C9 H12 Li N O3'
_chemical_formula_sum            'C9 H12 Li N O3'
_chemical_formula_weight         189.14
_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     direct
_audit_creation_date             2018-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-12 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                84.577(15)
_cell_angle_beta                 87.445(14)
_cell_angle_gamma                76.369(17)
_cell_formula_units_Z            2
_cell_length_a                   5.4312(10)
_cell_length_b                   7.6252(16)
_cell_length_c                   12.092(2)
_cell_measurement_reflns_used    809
_cell_measurement_temperature    153
_cell_measurement_theta_max      29.2934
_cell_measurement_theta_min      3.3532
_cell_volume                     484.37(16)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean 16.0727
_diffrn_measured_fraction_theta_full 0.9179
_diffrn_measured_fraction_theta_max 0.8932
_diffrn_measurement_details
;
  1 omega  -46.00   49.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4381   37.0000  120.0000 95

  2 omega  -89.00  -48.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4381  142.0000   40.0000 41

  3 omega  -72.00  -32.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4381  179.0000   90.0000 40

  4 omega  -90.00    5.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.4381  -37.0000  -60.0000 95
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0021963000
_diffrn_orient_matrix_UB_12      0.0306183000
_diffrn_orient_matrix_UB_13      -0.0572018000
_diffrn_orient_matrix_UB_21      0.0379054000
_diffrn_orient_matrix_UB_22      0.0781244000
_diffrn_orient_matrix_UB_23      0.0135042000
_diffrn_orient_matrix_UB_31      0.1289443000
_diffrn_orient_matrix_UB_32      -0.0467956000
_diffrn_orient_matrix_UB_33      -0.0044125000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2777
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.36
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47084
_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    1.2968
_exptl_crystal_description       block
_exptl_crystal_F_000             200.1140
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.3836
_refine_diff_density_min         -0.4085
_refine_diff_density_rms         0.0958
_refine_ls_d_res_high            0.7829
_refine_ls_d_res_low             6.0634
_refine_ls_goodness_of_fit_ref   1.0978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0978
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+0.0363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1939
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              9
_reflns_limit_k_min              -9
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                1145
_reflns_number_total             1891
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8cc08308h2.cif
_cod_data_source_block           RMG164
_cod_database_code               7122841
_reflns_odcompleteness_completeness 89.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
;
_olex2_submission_original_sample_id RMG164
_olex2_submission_special_instructions 'No special instructions were received'