3<i>H</i>-2,1-Benzoxaborole-1-spiro-4'-(5-oxa-3a-aza-4-borapyrene)
Robin, Beck; Buell, Gregg; Kiprof, Paul; Nemykin, Victor N.; Acta Crystallographica Section E 64 (2008) o314–o315; doi:10.1107/S1600536807066731

data_2217024
_publ_section_title
;
 3<i>H</i>-2,1-Benzoxaborole-1-spiro-4'-(5-oxa-3a-aza-4-borapyrene)
;
_journal_coeditor_code           EM2005
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o314
_journal_page_last               o315
_journal_paper_doi               10.1107/S1600536807066731
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C20 H14 B N O2'
_chemical_formula_moiety         'C20 H14 B N O2'
_chemical_formula_sum            'C20 H14 B N O2'
_chemical_formula_weight         311.13
_chemical_name_systematic
;
3<i>H</i>-2,1-Benzoxaborole-1-spiro-4'-(5-oxa-3a-aza-4-borapyrene)
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   33.079(5)
_cell_length_b                   33.079(5)
_cell_length_c                   7.358(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      18
_cell_measurement_theta_min      15
_cell_volume                     6973(5)
_computing_cell_refinement       'WinAFC (Rigaku/MSC, 2000)'
_computing_data_collection
'AFC-7R Diffractometer Control Software (Rigaku/MSC, 1997)'
_computing_data_reduction        'TEXSAN  (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>,  1996)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Rigaku AFC-7R'
_diffrn_measurement_device_type  Serial
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3564
_diffrn_reflns_theta_full        27.490
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         2.858
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2916
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.28
_refine_ls_extinction_coef       269(15)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0701
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     218
_refine_ls_number_reflns         1779
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1733
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.000267
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 6.52 6.79 1.78
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1346
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                1558
_reflns_number_total             3564
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            em2005.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2217024
_cod_database_fobs_code          2217024