The first report of the crystal structure of non-solvated μ-oxo boron subphthalocyanine and the crystal structures of two solvated forms
Fulford, Mabel V.; Lough, Alan John; Bender, Timothy P.; Acta Crystallographica Section B 68 (2012) 636–645; doi:10.1107/S0108768112037184

data_2105300
_publ_section_title
;
 The first report of the crystal structure of non-solvated \m-oxo boron
 subphthalocyanine and the crystal structures of two solvated forms
;
_journal_coeditor_code           RY5043
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              636
_journal_page_last               645
_journal_paper_doi               10.1107/S0108768112037184
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         'C48 H24 B2 N12 O, 0.25 (H2 O)'
_chemical_formula_sum            'C48 H24.5 B2 N12 O1.25'
_chemical_formula_weight         810.92
_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                87.5640(19)
_cell_angle_beta                 77.298(2)
_cell_angle_gamma                88.101(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4180(3)
_cell_length_b                   13.4413(6)
_cell_length_c                   13.9207(6)
_cell_measurement_reflns_used    35416
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.5
_cell_volume                     1899.35(13)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.1127
_diffrn_reflns_av_sigmaI/netI    0.1364
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35416
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         2.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.653
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             833
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.287
_refine_ls_extinction_coef       0.0094(17)
_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   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         8597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1864
_refine_ls_R_factor_gt           0.0666
_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^)+(0.1108P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.2136
_reflns_number_gt                3742
_reflns_number_total             8597
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ry5043.cif
_cod_data_source_block           H2O-m-oxo-BsubPc
_cod_original_formula_sum        'C48 H24.50 B2 N12 O1.25'
_cod_database_code               2105300