Intercepting low oxidation state main group hydrides with a nucleophilic N-hetereocyclic olefin
S.M. Ibrahim Al-Rafia; Adam Malcolm; Sean Liew; Michael Ferguson; Robert McDonald; Eri Rivard; Chem. Commun. 47 (2011) 6987–; doi:10.1039/c1cc11737h

data_7106532
_publ_section_title
;
 Intercepting low oxidation state main group hydrides with a nucleophilic
 N-hetereocyclic olefin
;
_journal_name_full               'Chem. Commun.'
_journal_page_first              6987
_journal_paper_doi               10.1039/c1cc11737h
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C28 H38 N2'
_chemical_formula_sum            'C28 H38 N2'
_chemical_formula_weight         402.60
_chemical_name_common            1
_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                79.6784(11)
_cell_angle_beta                 81.3389(12)
_cell_angle_gamma                78.5042(11)
_cell_formula_units_Z            8
_cell_length_a                   14.0622(12)
_cell_length_b                   16.6074(15)
_cell_length_c                   22.775(2)
_cell_measurement_reflns_used    5951
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.39
_cell_measurement_theta_min      2.27
_cell_volume                     5091.2(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w 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  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0921
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36469
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  0.9931
_exptl_absorpt_correction_T_min  0.9658
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0029(4)
_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   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         18420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1455
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0853P)^2^+0.3847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1921
_reflns_number_gt                9096
_reflns_number_total             18420
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1cc11737h.txt
_cod_data_source_block           riv1084
_cod_original_cell_volume        5091.3(8)
_cod_database_code               7106532