Hydrogen Elimination in Bulky Calcium Amidoborane Complexes: Isolation of a Calcium Borylamide Complex
Jan Spielmann; Sjoerd Harder; Journal of the American Chemical Society 131 (2009) 5064–5065; doi:10.1021/ja901073c

data_4104187
_publ_section_title
;
 Hydrogen Elimination in Bulky Calcium Amidoborane Complexes: Isolation of
 a Calcium Borylamide Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5064
_journal_page_last               5065
_journal_paper_doi               10.1021/ja901073c
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C68 H108 B2 Ca2 N6 O'
_chemical_formula_weight         1127.38
_chemical_name_common            '[(DIPP-nacnac)Ca]2(iPrN=BH-N(iPr)-BH3).THF'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.026(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9152(4)
_cell_length_b                   18.0011(6)
_cell_length_c                   31.6183(9)
_cell_measurement_temperature    123(2)
_cell_volume                     6777.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0845
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            112080
_diffrn_reflns_theta_full        24.76
_diffrn_reflns_theta_max         24.76
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.9789
_exptl_absorpt_correction_T_min  0.9585
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1144
_refine_ls_number_reflns         11553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0487P)^2^+2.2584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1144
_reflns_number_gt                8938
_reflns_number_total             11553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901073c_si_004.cif
_cod_data_source_block           hasj177
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4104187