Synthesis, Structure, and Bonding of Weakly Coordinating Anions Based on CN Adducts
Arne Bernsdorf; Harald Brand; Robert Hellmann; Martin Köckerling; Axel Schulz; Alexander Villinger; Karsten Voss; Journal of the American Chemical Society 131 (2009) 8958–8970; doi:10.1021/ja902450b

data_4104606
_publ_contact_author_address
;
Universit\"at Rostock
Institut f\"ur Chemie
Abteilung f\"ur Anorganische Chemie
Albert-Einstein-Strasse 3a 
18059 Rostock
Bundesrepublik Deutschland
;
_publ_contact_author_email       axel.schulz@uni-rostock.de
_publ_contact_author_fax         '+49 (0)381/498-6382'
_publ_contact_author_name        'Axel Schulz'
_publ_contact_author_phone       '+49 (0)381/498-6400'
_publ_section_title
;
 Synthesis, Structure, and Bonding of Weakly Coordinating Anions Based on
 CN Adducts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8958
_journal_page_last               8970
_journal_paper_doi               10.1021/ja902450b
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety
'C58 B3 F45 N3 -, K C12 H24 O3 +, C1.82 H4.38 O0.46'
_chemical_formula_sum            'C71.82 H28.38 B3 F45 K N3 O6.46'
_chemical_formula_weight         1963.11
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.15(3)
_cell_angle_beta                 81.19(3)
_cell_angle_gamma                71.50(3)
_cell_formula_units_Z            4
_cell_length_a                   18.433(4)
_cell_length_b                   19.776(4)
_cell_length_c                   24.987(5)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      53.608
_cell_measurement_theta_min      4.657
_cell_volume                     8011(4)
_computing_cell_refinement       'Bruker Apex v2.0-2'
_computing_data_collection       'Bruker Apex v2.0-2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            114777
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  0.9255
_exptl_absorpt_correction_T_min  0.9057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       block
_exptl_crystal_F_000             3884
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2629
_refine_ls_number_reflns         28083
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0898P)^2^+4.0565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1808
_reflns_number_gt                18592
_reflns_number_total             28083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja902450b_si_002.cif
_cod_data_source_block           k_tcm
_cod_original_cell_volume        8011(3)
_cod_database_code               4104606