Ionic-Type Reactivity of 1,3-Dibora-2,4-diphosphoniocyclobutane-1,3-diyls: Regio- and Stereoselective Addition of Hydracids
Gad Fuks; Nathalie Saffon; Laurent Maron; Guy Bertrand; Didier Bourissou; Journal of the American Chemical Society 131 (2009) 13681–13689; doi:10.1021/ja903746p

data_4105059
_publ_section_title
;
 Ionic-Type Reactivity of
 1,3-Dibora-2,4-diphosphoniocyclobutane-1,3-diyls: Regio- and
 Stereoselective Addition of Hydracids
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13681
_journal_page_last               13689
_journal_paper_doi               10.1021/ja903746p
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C44 H86 B4 Cl2 P4'
_chemical_formula_weight         853.15
_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                67.4280(10)
_cell_angle_beta                 88.6680(10)
_cell_angle_gamma                87.4890(10)
_cell_formula_units_Z            2
_cell_length_a                   13.1771(10)
_cell_length_b                   14.2465(11)
_cell_length_c                   14.6210(11)
_cell_measurement_reflns_used    6503
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.114
_cell_measurement_theta_min      2.148
_cell_volume                     2532.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17763
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_T_max  0.9916
_exptl_absorpt_correction_T_min  0.8053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            'lustrous intense colourless'
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         8463
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0437P)^2^+1.0440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                6544
_reflns_number_total             8463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903746p_si_003.cif
_cod_data_source_block           gad03m
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_database_code               4105059