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_4104186
_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            'C36 H60 B Ca N3 O'
_chemical_formula_weight         601.76
_chemical_name_common            DIPP-nacnac)CaN(DIPP)H-BH3.THF
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2b'
_symmetry_space_group_name_H-M   'P b n a'
_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            8
_cell_length_a                   16.5823(15)
_cell_length_b                   17.0572(15)
_cell_length_c                   26.097(3)
_cell_measurement_temperature    173(2)
_cell_volume                     7381.5(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0940
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            269701
_diffrn_reflns_theta_full        29.62
_diffrn_reflns_theta_max         29.62
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.9426
_exptl_absorpt_correction_T_min  0.9069
_exptl_absorpt_correction_type   emprirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         10356
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0785
_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^)+(0.0745P)^2^+6.4512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1813
_refine_ls_wR_factor_ref         0.1921
_reflns_number_gt                8336
_reflns_number_total             10356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901073c_si_003.cif
_cod_data_source_block           hasj166
_cod_original_cell_volume        7381.4(12)
_cod_original_sg_symbol_H-M      Pbna
_cod_database_code               4104186