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_4337171
_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            'C24 H64 B4 Ca N2 O9'
_chemical_formula_weight         608.09
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.528(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7631(10)
_cell_length_b                   10.1952(6)
_cell_length_c                   23.2794(15)
_cell_measurement_temperature    193(2)
_cell_volume                     3621.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1510
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55374
_diffrn_reflns_theta_full        27.21
_diffrn_reflns_theta_max         27.21
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.217
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         8018
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1243
_reflns_number_gt                4861
_reflns_number_total             8018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402237b_si_002.cif
_cod_data_source_block           ba23l_14face
_cod_database_code               4337171