Synthesis and Structural Diversity of Barium (N,N-Dimethylamino)diboranates
Scott R. Daly; Brian J. Bellott; Mark A. Nesbit; Gregory S. Girolami; Inorganic Chemistry 51 (2012) 6449–6459; doi:10.1021/ic2016879

data_4329404
_publ_section_title
;
 Synthesis and Structural Diversity of Barium
 (N,N-Dimethylamino)diboranates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6449
_journal_page_last               6459
_journal_paper_doi               10.1021/ic2016879
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C13 H47 B4 Ba N5'
_chemical_formula_weight         454.13
_chemical_name_systematic
; 
 ? 
;
_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                 95.937(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.544(3)
_cell_length_b                   18.799(6)
_cell_length_c                   14.610(5)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      1.77
_cell_volume                     2607.2(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.1400
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6519
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.527
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.042
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.751
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4479
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.753
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                2345
_reflns_number_total             4479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2016879_si_002_07.cif
_cod_data_source_block           f59kf_14face
_cod_original_cell_volume        2607.2(14)
_cod_database_code               4329404