Synthesis and Characterization of New 19-Vertex Macropolyhedral Boron Hydrides
Joel A. Dopke; Douglas R. Powell; Donald F. Gaines; Inorganic Chemistry 39 (2000) 463–467; doi:10.1021/ic990896c

data_4300142
_publ_contact_author
; 
    Prof. Donald F. Gaines 
    Department of Chemistry 
    University of Wisconsin 
    Madison, WI  53706-1396  USA 
;
_publ_contact_author_email       gaines@chem.wisc.edu
_publ_contact_author_fax         1(608)2620381
_publ_contact_author_phone       1(608)2625806
_publ_section_title
;
Synthesis and Characterization of New 19-Vertex Macropolyhedral Boron
Hydrides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              463
_journal_page_last               467
_journal_paper_doi               10.1021/ic990896c
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         '(C36 H30 N P2)+ (B19 H20)- 0.5(C4 H8 O)'
_chemical_formula_sum            'C38 H54 B19 N O0.5 P2'
_chemical_formula_weight         800.15
_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                77.402(2)
_cell_angle_beta                 81.351(2)
_cell_angle_gamma                73.253(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6344(2)
_cell_length_b                   13.5978(2)
_cell_length_c                   14.1401(2)
_cell_measurement_reflns_used    6450
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     2260.25(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_device       'Siemens P4/ccd'
_diffrn_measurement_method       'phi scan frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25142
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        -0.12
_diffrn_standards_number         286
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         10670
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.141
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1002P)^2^+0.3620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.1934
_reflns_number_gt                6940
_reflns_number_total             10670
_reflns_threshold_expression     >2sigma(I)
_cod_original_formula_sum        'C38 H54 B19 N O0.50 P2'
_cod_database_code               4300142