Diverse chemistry of the dianion [closo-B9H9]2−: synthesis and reactivity of its mono-anionic derivative [arachno-B9H12-4,8-Cl2]−
Schlüter, Florian; Bernhardt, Eduard; Zhizhin, Konstantin; New Journal of Chemistry 42 (2018) 2553–; doi:10.1039/C7NJ04251E

data_7056936
_publ_section_title
;
 Diverse chemistry of the dianion [closo-B9H9]2&#x2212;: synthesis and
 reactivity of its mono-anionic derivative [arachno-B9H12-4,8-Cl2]&#x2212;
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2553
_journal_paper_doi               10.1039/C7NJ04251E
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C24 H32.04 B9 Cl2.04 P'
_chemical_formula_weight         521.25
_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_method           SHELXL-2013
_audit_update_record
;
2017-08-19 deposited with the CCDC.
2018-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.776(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.2777(7)
_cell_length_b                   10.3096(2)
_cell_length_c                   25.1059(8)
_cell_measurement_reflns_used    15211
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.7716
_cell_measurement_theta_min      3.1290
_cell_volume                     5633.2(3)
_computing_cell_refinement       'CrysAlisPro171.36.24, Oxford Diffraction'
_computing_data_collection       'CrysAlisPro171.36.24, Oxford Diffraction'
_computing_data_reduction        'CrysAlisPro171.36.24, Oxford Diffraction'
_computing_molecular_graphics    'Diamond, v.2.1e (Brandenburg, 2001)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type
'Gemini E Ultra,Xcalibur,2K*2K EOS CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube Enhanced (Mo)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            34405
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        30.500
_diffrn_reflns_theta_max         32.846
_diffrn_reflns_theta_min         3.135
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       prism
_exptl_crystal_F_000             2166
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichlormethane/Pentane'
_exptl_crystal_size_max          0.4845
_exptl_crystal_size_mid          0.3255
_exptl_crystal_size_min          0.2711
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         9556
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0451P)^2^+3.4235P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8359
_reflns_number_total             9556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj04251e2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments          'Adding full bibliography for 7056936.cif.'
_cod_database_code               7056936
_shelxl_version_number           2013-2
_shelx_res_checksum              17172