Molten metal closo-borate solvates
Møller, Kasper T.; Paskevicius, Mark; Andreasen, Jacob Ginnerup; Lee, Junqiao; Chen-Tan, Nigel; Overgaard, Jacob; Payandeh, Seyedhosein; Silvester, Debbie S.; Buckley, Craig; Jensen, Torben Rene R.; Chemical Communications  (2019) –; doi:10.1039/C9CC00187E

data_7123054
_publ_section_title
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 Molten metal closo-borate solvates
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00187E
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C8 H12 Li N4, 0.5(B12 H12)'
_chemical_formula_sum            'C8 H18 B6 Li N4'
_chemical_formula_weight         242.06
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-12-04 deposited with the CCDC.    2019-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.0374(4)
_cell_length_b                   10.0374(4)
_cell_length_c                   31.778(2)
_cell_measurement_reflns_used    2951
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.2130
_cell_measurement_theta_min      3.2550
_cell_volume                     3201.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3590
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     34.00  85.00   1.00   30.00    --   10.84-178.00 120.00   51
  2  \w    -36.00  32.00   1.00   30.00    --   10.84 -77.00 -60.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0127460000
_diffrn_orient_matrix_UB_12      0.0092358000
_diffrn_orient_matrix_UB_13      -0.0217573000
_diffrn_orient_matrix_UB_21      -0.0058865000
_diffrn_orient_matrix_UB_22      -0.0695955000
_diffrn_orient_matrix_UB_23      -0.0032872000
_diffrn_orient_matrix_UB_31      -0.0693052000
_diffrn_orient_matrix_UB_32      0.0076783000
_diffrn_orient_matrix_UB_33      -0.0037118000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            10789
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.201
_diffrn_reflns_theta_min         2.400
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.056
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.004
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1016
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 880 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0475P)^2^+0.2020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.602
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.814
_reflns_number_gt                2949
_reflns_number_total             3814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00187e2.cif
_cod_data_source_block           exp_304
_cod_database_code               7123054
_chemical_oxdiff_formula         C8H18B6LiN4
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C008(H00A,H00B,H00C), C00A(H00D,H00E,H00F), C00B(H00G,H00H,H00I), C00C(H00J,
 H00K,H00L)
2.b Boron cage BH refined with riding coordinates:
 B00D(H00M), B00E(H00N), B00F(H00O), B00G(H00P), B00H(H00Q), B00I(H00R)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2017-04-28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.241
_oxdiff_exptl_absorpt_empirical_full_min 0.793