New Syntheses and Structural Characterization of NH3BH2Cl and (BH2NH2)3 and Thermal Decomposition Behavior of NH3BH2Cl
Hima K. Lingam; Cong Wang; Judith C. Gallucci; Xuenian Chen; Sheldon G. Shore; Inorganic Chemistry 51 (2012) 13430–13436; doi:10.1021/ic302308v

data_4331381
_publ_contact_author_address
;
Department of Chemistry & Biochemistry
100 W 18th Avenue
Columbus OH 43220
;
_publ_contact_author_email       shore.1@osu.edu
_publ_contact_author_fax         (614)-292-1685
_publ_contact_author_name        'Sheldon G Shore'
_publ_contact_author_phone       (614)-292-6000
_publ_section_title
;
 New Syntheses and Structural Characterization of NH3BH2Cl and (BH2NH2)3
 and Thermal Decomposition Behavior of NH3BH2Cl
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13430
_journal_page_last               13436
_journal_paper_doi               10.1021/ic302308v
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'B3 H12 N3'
_chemical_formula_sum            'B3 H12 N3'
_chemical_formula_weight         86.56
_chemical_name_common            cyclotriborazane
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-10-19 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.383(2)
_cell_length_b                   12.193(2)
_cell_length_c                   11.180(2)
_cell_measurement_reflns_used    1256
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.34
_cell_volume                     597.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'PHI SCANS & 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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1256
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    0.058
_exptl_absorpt_correction_T_max  0.9914
_exptl_absorpt_correction_T_min  0.9801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL SCALEPACK (OTWINOWSKI & MINOR, 1997)'
_exptl_crystal_density_diffrn    0.962
_exptl_crystal_F_000             192
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1144
_reflns_number_gt                441
_reflns_number_total             722
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302308v_si_002_3.cif
_cod_data_source_block           shore1837
_cod_database_code               4331381