Synthesis and characterization of calcium n,n-dimethylaminodiboranates as possible chemical vapor deposition precursors.
Dunbar, Andrew C.; Girolami, Gregory S.; Inorganic chemistry 53 (2014) 888–896; doi:10.1021/ic402237b

data_4337170
_publ_section_title
;
 Synthesis and characterization of calcium n,n-dimethylaminodiboranates as
 possible chemical vapor deposition precursors.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              888
_journal_page_last               896
_journal_paper_doi               10.1021/ic402237b
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C10 H40 B4 Ca N4'
_chemical_formula_weight         299.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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                 97.201(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1637(6)
_cell_length_b                   14.9076(9)
_cell_length_c                   13.7731(8)
_cell_measurement_reflns_used    5645
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.17
_cell_measurement_theta_min      2.45
_cell_volume                     2070.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1179
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39094
_diffrn_reflns_theta_full        27.17
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.962
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.222
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4583
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1285
_reflns_number_gt                3084
_reflns_number_total             4583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402237b_si_002.cif
_cod_data_source_block           ba67i_p21n_face
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4337170