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_4329407
_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            'C30 H84 B6 Ba N3 Na O10'
_chemical_formula_weight         872.19
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                60.409(2)
_cell_angle_beta                 89.888(3)
_cell_angle_gamma                72.825(3)
_cell_formula_units_Z            4
_cell_length_a                   12.7000(7)
_cell_length_b                   21.3688(11)
_cell_length_c                   21.5299(11)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.19
_cell_measurement_theta_min      2.20
_cell_volume                     4780.9(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1408
_diffrn_reflns_av_sigmaI/netI    0.1119
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            92516
_diffrn_reflns_theta_full        27.31
_diffrn_reflns_theta_max         27.31
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  0.8841
_exptl_absorpt_correction_T_min  0.6521
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       prism
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.784
_exptl_crystal_size_mid          0.296
_exptl_crystal_size_min          0.289
_refine_diff_density_max         2.188
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1403
_refine_ls_number_reflns         21327
_refine_ls_number_restraints     2079
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                12684
_reflns_number_total             21327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2016879_si_002_10.cif
_cod_data_source_block           fa66kface
_cod_original_cell_volume        4780.9(4)
_cod_database_code               4329407