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_2105301
_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, 2(C6 H4 Cl2)'
_chemical_formula_sum            'C60 H32 B2 Cl4 N12 O'
_chemical_formula_weight         1100.40
_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                78.3470(16)
_cell_angle_beta                 85.6160(13)
_cell_angle_gamma                76.7400(17)
_cell_formula_units_Z            2
_cell_length_a                   11.3894(3)
_cell_length_b                   13.2623(3)
_cell_length_c                   17.6618(6)
_cell_measurement_reflns_used    25833
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     2541.89(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 0.989
_diffrn_measured_fraction_theta_max 0.973
_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  0.0758
_diffrn_reflns_av_sigmaI/netI    0.1088
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26858
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.808
_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    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.495
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         11383
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1671
_refine_ls_R_factor_gt           0.0848
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+4.0961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.2170
_reflns_number_gt                6168
_reflns_number_total             11383
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ry5043.cif
_cod_data_source_block           DCB-m-oxo-BsubPc
_cod_original_cell_volume        2541.89(12)
_cod_database_code               2105301