Molecular Hydrogen Tweezers: Structure and Mechanisms by Neutron Diffraction, NMR, and Deuterium Labeling Studies in Solid and Solution
Felix Schulz; Victor Sumerin; Sami Heikkinen; Björn Pedersen; Cong Wang; Michiko Atsumi; Markku Leskelä; Timo Repo; Pekka Pyykkö; Winfried Petry; Bernhard Rieger; Journal of the American Chemical Society 133 (2011) 20245–20257; doi:10.1021/ja206394w

data_4107212
_publ_contact_author_address
;   Department of Chemistry
    University of Helsinki 
    P.O. Box 55
    FIN-00014 Helsinki 
    Finland
;
_publ_contact_author_email       timo.repo@helsinki.fi
_publ_contact_author_fax         '+358 9 191 50198'
_publ_contact_author_name        '   Prof. Dr. Timo Repo'
_publ_contact_author_phone       '+358 9 191 50194'
_publ_section_title
;
 Molecular Hydrogen Tweezers: Structure and Mechanisms by Neutron
 Diffraction, NMR, and Deuterium Labeling Studies in Solid and Solution
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20245
_journal_page_last               20257
_journal_paper_doi               10.1021/ja206394w
_journal_volume                  133
_journal_year                    2011
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C28 H26 B F10 N, 0.5(C6 D6)'
_chemical_formula_sum            'C31 H26 B D3 F10 N'
_chemical_formula_weight         619.37
_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   ' ?'
_atom_sites_solution_primary     ' ?'
_atom_sites_solution_secondary   ' ?'
_audit_creation_date             'Aug 26 09:40:03 2011'
_audit_creation_method           'PLATON <TABLE ACC> option'
_cell_angle_alpha                86.77(5)
_cell_angle_beta                 70.73(5)
_cell_angle_gamma                64.83(5)
_cell_formula_units_Z            2
_cell_length_a                   10.587(10)
_cell_length_b                   12.183(10)
_cell_length_c                   12.52(1)
_cell_measurement_reflns_used    9010
_cell_measurement_temperature    10
_cell_measurement_theta_max      35
_cell_measurement_theta_min      4
_cell_volume                     1373(2)
_computing_cell_refinement
'peakref (Duisenberg, Kron-Baatenburg & Schreurs, 2003)'
_computing_data_collection
'Bruker-Nonius Collect Bruker, 2007), locally modified'
_computing_data_reduction
'EVAL14 (Duisenberg, Kron-Baatenburg & Schreurs, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  JANA2000
_diffrn_ambient_temperature      10
_diffrn_detector_area_resol_mean 18.4
_diffrn_measured_fraction_theta_full 0.4
_diffrn_measured_fraction_theta_max 0.59
_diffrn_measurement_device_type  Mar345+FujiBasND
_diffrn_measurement_method       'roation method'
_diffrn_radiation_monochromator  Cu-422
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'FRM II'
_diffrn_radiation_wavelength     1.03000
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9015
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        40.1
_diffrn_reflns_theta_max         49
_diffrn_reflns_theta_min         4
_exptl_absorpt_coefficient_mu    0.004
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   'integration from crystal shape'
_exptl_crystal_colour            'clear, colourless'
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             0
_exptl_crystal_size_max          2
_exptl_crystal_size_mid          2
_exptl_crystal_size_min          2
_refine_diff_density_max         1.560
_refine_diff_density_min         -1.400
_refine_ls_extinction_coef       88(2)
_refine_ls_extinction_method     'b-c type 1 lorent'
_refine_ls_goodness_of_fit_ref   1.420
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         9015
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     W=1/(\S^2^(F)+0.0001F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                5332
_reflns_number_total             9015
_reflns_threshold_expression     i>2.5\s(i)
_cod_data_source_file            ja206394w_si_001.cif
_cod_data_source_block           global
_cod_original_formula_sum        'C31 H26 B1 D3 F10 N1'
_cod_database_code               4107212