Mononuclear Schiff Base Boron Halides: Synthesis, Characterization, and Dealkylation of Trimethyl Phosphate
Mitra, Amitabha; DePue, Lauren J.; Struss, Jeffrey E.; Patel, Bijal P.; Parkin, Sean; Atwood, David A.; Inorganic Chemistry 45 (2006) 9213–9224; doi:10.1021/ic0607890

data_4332745
_publ_section_title
;
 Mononuclear Schiff Base Boron Halides:&#x00A0; Synthesis,
 Characterization, and Dealkylation of Trimethyl Phosphate
;
_journal_issue                   23
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9213
_journal_page_last               9224
_journal_paper_doi               10.1021/ic0607890
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C18 H27 B Br N O2'
_chemical_formula_weight         380.13
_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                101.1731(3)
_cell_angle_beta                 101.3603(4)
_cell_angle_gamma                115.8035(3)
_cell_formula_units_Z            4
_cell_length_a                   11.5811(1)
_cell_length_b                   11.9058(1)
_cell_length_c                   16.5674(1)
_cell_measurement_reflns_used    8655
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1912.52(3)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1994)'
_computing_publication_material
; 
SHELX97-2 (Sheldrick, 1997) and local procedures 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47040
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    2.157
_exptl_absorpt_correction_T_max  0.8463
_exptl_absorpt_correction_T_min  0.5638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         .408
_refine_diff_density_min         -.409
_refine_diff_density_rms         .059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         8775
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.081
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.9709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                7220
_reflns_number_total             8775
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic0607890sup4.cif
_cod_data_source_block           k05183
_cod_database_code               4332745