Dynamic Disorder and Electronic Structures of Electron-Precise Dianionic Diboranes: Insights from Solid-State Multinuclear Magnetic Resonance Spectroscopy.
Wong, Y. T. Angel; Landmann, Johannes; Finze, Maik; Bryce, David L.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b01783

data_4126197
_publ_section_title
;
 Dynamic Disorder and Electronic Structures of Electron-Precise Dianionic
 Diboranes: Insights from Solid-State Multinuclear Magnetic Resonance
 Spectroscopy.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b01783
_journal_year                    2017
_chemical_formula_moiety         'C12 H36 Cu O6 S6, C6 B2 N6'
_chemical_formula_sum            'C18 H36 B2 Cu N6 O6 S6'
_chemical_formula_weight         710.05
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
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_cell_angle_beta                 90
_cell_angle_gamma                120
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_cell_length_b                   14.0349(13)
_cell_length_c                   15.6390(15)
_cell_measurement_reflns_used    1921
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.99
_cell_measurement_theta_min      2.90
_cell_volume                     2667.8(4)
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
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_diffrn_detector                 'CCD area detector (Apex2)'
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_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
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_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.754
_diffrn_reflns_theta_min         2.122
_diffrn_source                   'rotating-anode (Nonius FR-591)'
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_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_crystal_colour            blue
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_exptl_crystal_description       block
_exptl_crystal_F_000             1107
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0348P)^2^+11.5925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                899
_reflns_number_total             1269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b01783_si_002.cif
_cod_data_source_block           CuDMSO6B2CN6
_cod_original_cell_volume        2667.8(6)
_cod_database_code               4126197
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              48321
_shelx_hkl_checksum              76227