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_7123053
_publ_section_title
;
 Molten metal closo-borate solvates
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00187E
_journal_year                    2019
_chemical_formula_moiety         'C12 H30 B6 Li O3'
_chemical_formula_sum            'C12 H30 B6 Li O3'
_chemical_formula_weight         294.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-03-09
_audit_creation_method           'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_audit_update_record
;
2018-12-04 deposited with the CCDC.    2019-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 111.270(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   14.7037(4)
_cell_length_b                   14.1409(3)
_cell_length_c                   18.2503(4)
_cell_measurement_reflns_used    5015
_cell_measurement_temperature    100.02(16)
_cell_measurement_theta_max      28.1480
_cell_measurement_theta_min      2.0560
_cell_volume                     3536.18(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (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      100.02(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3590
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.895
_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    -82.00  62.00   1.00   60.00    --   18.53 -77.00 120.00  144
  2  \w   -112.00  22.00   1.00   60.00    --  -19.62 -57.00 -30.00  134
  3  \w    -65.00 -31.00   1.00   60.00    --  -19.62  39.00  -6.00   34
;
_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      0.0469439000
_diffrn_orient_matrix_UB_12      0.0052686000
_diffrn_orient_matrix_UB_13      -0.0021019000
_diffrn_orient_matrix_UB_21      0.0058473000
_diffrn_orient_matrix_UB_22      0.0436597000
_diffrn_orient_matrix_UB_23      0.0203636000
_diffrn_orient_matrix_UB_31      0.0209745000
_diffrn_orient_matrix_UB_32      -0.0241309000
_diffrn_orient_matrix_UB_33      0.0363471000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11198
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.590
_diffrn_reflns_theta_min         2.070
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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    1.105
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1272
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Tetrahydrofuran'
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0687P)^2^+4.4038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3345
_reflns_number_total             4057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00187e2.cif
_cod_data_source_block           exp_282
_cod_original_cell_volume        3536.19(14)
_cod_database_code               7123053
_chemical_oxdiff_formula         'B12 H12 Li2 (C4 O H8)6'
_cell_oxdiff_angle_alpha         90.057(4)
_cell_oxdiff_angle_beta          111.260(4)
_cell_oxdiff_angle_gamma         89.907(4)
_cell_oxdiff_length_a            14.7079(8)
_cell_oxdiff_length_b            14.1402(7)
_cell_oxdiff_length_c            18.2449(8)
_cell_oxdiff_measurement_reflns_used 5018
_cell_oxdiff_volume              3536.2(3)
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Sof(H24C)=Sof(H24D)=Sof(C22)=Sof(H22A)=Sof(H22B)=1-FVAR(1)
 Sof(H24A)=Sof(H24B)=Sof(C23)=Sof(H23A)=Sof(H23B)=FVAR(1)
 Sof(C32)=Sof(H32A)=Sof(H32B)=1-FVAR(2)
 Sof(C31)=Sof(H31A)=Sof(H31B)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C21(H21A,H21B), C4(H4A,H4B), C3(H3A,H3B), C34(H34A,H34B),
 C2(H2A,H2B), C31(H31A,H31B), C24(H24A,H24B), C24(H24C,H24D), C35(H35A,H35B),
 C1(H1A,H1B), C33(H33A,H33B), C23(H23A,H23B), C22(H22A,H22B), C32(H32A,H32B)
3.b Boron cage BH refined with riding coordinates:
 B4(H4), B5(H5), B3(H3)
;
_shelx_res_checksum              12456
_shelx_hkl_checksum              5636
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2017-03-07
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.288
_oxdiff_exptl_absorpt_empirical_full_min 0.861