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_4104184
_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            'C45 H68 B Ca N3 O'
_chemical_formula_weight         2871.66
_chemical_name_common            (DIPP-nacnac)Ca(DIPP)N=BH2.THF
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1390(3)
_cell_length_b                   18.6226(4)
_cell_length_c                   21.2712(5)
_cell_measurement_temperature    133(2)
_cell_volume                     4412.44(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81060
_diffrn_reflns_theta_full        28.94
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.9684
_exptl_absorpt_correction_T_min  0.9432
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         5952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0526P)^2^+1.3914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1144
_reflns_number_gt                4879
_reflns_number_total             5952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901073c_si_001.cif
_cod_data_source_block           hasj140
_cod_original_sg_symbol_H-M      Pbcm
_cod_original_formula_sum        'C45 H68 B1 Ca1 N3 O1'
_cod_database_code               4104184