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_4332746
_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_moiety         'C42 H50 B2 N2 O5, 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H54 B2 Cl4 N2 O5'
_chemical_formula_weight         854.31
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   12.9606(2)
_cell_length_b                   19.6141(3)
_cell_length_c                   51.9064(7)
_cell_measurement_reflns_used    7798
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      67.35
_cell_measurement_theta_min      3.46
_cell_volume                     13195.2(3)
_computing_cell_refinement       'APEX2 (Bruker-Nonius, 2004)'
_computing_data_collection       'APEX2 (Bruker-Nonius, 2004)'
_computing_data_reduction        'APEX2 (Bruker-Nonius, 2004)'
_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 .989
_diffrn_measured_fraction_theta_max .989
_diffrn_measurement_device_type  'X8 Proteum diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Bruker Montel multilayer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            93693
_diffrn_reflns_theta_full        67.99
_diffrn_reflns_theta_max         67.99
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    2.810
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs in APEX2 (Bruker-Nonius, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shard'
_exptl_crystal_F_000             5400
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         .636
_refine_diff_density_min         -2.050
_refine_diff_density_rms         .069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(15)
_refine_ls_extinction_coef       0.000089(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1658
_refine_ls_number_reflns         23333
_refine_ls_number_restraints     2722
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+12.8198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1947
_reflns_number_gt                16374
_reflns_number_total             23333
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic0607890sup5.cif
_cod_data_source_block           x04051
_cod_database_code               4332746