Intramolecular base-stabilised adducts of main group halides
Aldridge, Simon; Calder, Richard J.; Coombs, Deborah L.; Jones, Cameron; Steed, Jonathan W.; Coles, Simon; Hursthouse, Michael B.; New Journal of Chemistry 26 (2002) 677–; doi:10.1039/b110692a

data_7050794
_publ_section_title
;
 Intramolecular base-stabilised adducts of main group halides
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              677
_journal_paper_doi               10.1039/b110692a
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C9 H15 B Br2 N2 Si'
_chemical_formula_weight         349.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.113(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.8246(7)
_cell_length_b                   13.9297(17)
_cell_length_c                   14.2729(17)
_cell_measurement_temperature    100(2)
_cell_volume                     1354.8(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'XSeed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '2o phi+omega frames 5s deg-1'
_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  0.1559
_diffrn_reflns_av_sigmaI/netI    0.1351
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6753
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.33
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.043
_exptl_absorpt_correction_T_max  0.1960
_exptl_absorpt_correction_T_min  0.0856
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.645
_refine_diff_density_min         -1.401
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       0.0099(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2643
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0192P)^2^+5.7537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                2102
_reflns_number_total             2643
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110692a.txt
_cod_data_source_block           sa3
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7050794