Synthesis and characterization of synthetically useful salts of the weakly-coordinating dianion [B12Cl12]2−
Geis, Vanessa; Guttsche, Kristin; Knapp, Carsten; Scherer, Harald; Uzun, Rabiya; Dalton Transactions  (2009) 2687–2694; doi:10.1039/b821030f

data_7000986
_publ_section_title
;
 Synthesis and characterization of synthetically useful salts of the
 weakly-coordinating dianion [B12Cl12]2&#x2212;
;
_journal_issue                   15
_journal_name_full               'Dalton Transactions'
_journal_page_first              2687
_journal_page_last               2694
_journal_paper_doi               10.1039/b821030f
_journal_year                    2009
_chemical_formula_moiety         '2(C19 H15), (B12 Cl12), 2(O2 S)'
_chemical_formula_sum            'C38 H30 B12 Cl12 O4 S2'
_chemical_formula_weight         1169.86
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.205(3)
_cell_length_b                   16.617(3)
_cell_length_c                   19.010(4)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      0.00
_cell_volume                     4995.7(18)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
scan:
Number of images: 90
Slice: 20.0000 - 200.0000
Image width: 2.0000
Exp time: 138.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 15.0000
Phi: 0.0000
XTD: 127.4000
2theta: 0.0000
scan:
Number of images: 54
Slice: 74.0000 - 182.0000
Image width: 2.0000
Exp time: 138.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 15.0000
Phi: 180.0000
XTD: 127.4000
2theta: 0.0000
scan:
Number of images: 22
Slice: 108.0000 - 152.0000
Image width: 2.0000
Exp time: 138.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 15.0000
Phi: 90.0000
XTD: 127.4000
2theta: 0.0000
scan:
Number of images: 15
Slice: 30.0000 - 60.0000
Image width: 2.0000
Exp time: 138.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 0.0000
Phi: 270.0000
XTD: 127.4000
2theta: 0.0000
scan:
Number of images: 15
Slice: 40.0000 - 70.0000
Image width: 2.0000
Exp time: 138.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 15.0000
Phi: 270.0000
XTD: 127.4000
2theta: 0.0000
;
_diffrn_measurement_device_type  'Rigaku R-AXIS Spider'
_diffrn_measurement_method       fsFind.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43480
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
March 2001 T Higashi
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+5.5202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                4697
_reflns_number_total             5725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b821030f.txt
_cod_data_source_block           ck001
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4995.8(17)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7000986