Molecular Tweezers for Hydrogen: Synthesis, Characterization, and Reactivity
Victor Sumerin; Felix Schulz; Michiko Atsumi; Cong Wang; Martin Nieger; Markku Leskelä; Timo Repo; Pekka Pyykkö; Bernhard Rieger; Journal of the American Chemical Society 130 (2008) 14117–14119; doi:10.1021/ja806627s

data_4108573
_publ_contact_author
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        Martin Nieger
        Laboratory of Inorganic Chemistry
        Department of Chemistry
        Universitity of Helsinki
        P.O. Box 55
        FIN-00014 University of Helsinki
        Finland
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_publ_contact_author_email       martin.nieger@helsinki.fi
_publ_contact_author_fax         ++358-9-19150198
_publ_contact_author_phone       ++358-9-19150223
_publ_section_title
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 Molecular Tweezers for Hydrogen: Synthesis, Characterization, and
 Reactivity
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14117
_journal_page_last               14119
_journal_paper_doi               10.1021/ja806627s
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C28 H26 B F10 N, 0.5 (C6 D6)'
_chemical_formula_sum            'C31 H26 B D3 F10 N'
_chemical_formula_weight         619.38
_chemical_name_systematic
; 
 Hydrido[bis(pentafluorophenyl){2-[(2,2,6,6-tetramethylpiperidinium-1-yl)-
 methyl]phenyl}borate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                86.96(1)
_cell_angle_beta                 70.73(1)
_cell_angle_gamma                65.17(1)
_cell_formula_units_Z            2
_cell_length_a                   10.652(1)
_cell_length_b                   12.256(1)
_cell_length_c                   12.595(1)
_cell_measurement_reflns_used    96
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     1401.6(3)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'EVALCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 2 deg.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13264
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plates
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         4922
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0416P)^2^+0.8714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                3845
_reflns_number_total             4922
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806627s_si_002.cif
_cod_data_source_block           les045_d_compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1401.6(2)
_cod_database_code               4108573