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_4104185
_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 H70 B Ca N3 O'
_chemical_formula_weight         719.93
_chemical_name_common            (DIPP-nacnac)Ca(NH(DIPP)BH3).THF
_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                 106.287(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9746(6)
_cell_length_b                   22.8411(12)
_cell_length_c                   17.0308(8)
_cell_measurement_temperature    173(2)
_cell_volume                     4471.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.1283
_diffrn_reflns_av_sigmaI/netI    0.0786
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            94907
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.9894
_exptl_absorpt_correction_T_min  0.9518
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            light_green
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         10191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+2.6462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                6687
_reflns_number_total             10191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901073c_si_002.cif
_cod_data_source_block           hasj148
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4104185