Borylated porphyrins: 5,10,15,20-tetrakis(5,5-dimethyl-1,3,2-dioxaborinan-2-yl)porphyrin nitrobenzene disolvate
Muniappan, Sankar; Lipstman, Sophia; Goldberg, Israel; Acta Crystallographica Section C 64 (2008) o177–o179; doi:10.1107/S010827010800468X

data_2016509
_publ_section_title
;
 Borylated porphyrins:
 5,10,15,20-tetrakis(5,5-dimethyl-1,3,2-dioxaborinan-2-yl)porphyrin
 nitrobenzene disolvate
;
_journal_coeditor_code           SF3072
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o177
_journal_page_last               o179
_journal_paper_doi               10.1107/S010827010800468X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C64 H66 B4 N4 O8, 2C6 H5 N O2'
_chemical_formula_moiety         'C64 H66 B4 N4 O8, 2(C6 H5 N O2)'
_chemical_formula_sum            'C76 H76 B4 N6 O12'
_chemical_formula_weight         1308.67
_chemical_name_systematic
;
5,10,15,20-tetrakis(5,5-dimethyl-1,3,2-dioxaborinan-2-yl)porphyrin
nitrobenzene clathrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 110.1016(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.6511(7)
_cell_length_b                   9.2969(3)
_cell_length_c                   20.7606(9)
_cell_measurement_reflns_used    6670
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.60
_cell_measurement_theta_min      2.09
_cell_volume                     3380.5(2)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1\% \f and \w'
_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  0.0892
_diffrn_reflns_av_sigmaI/netI    0.1061
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23064
_diffrn_reflns_theta_full        25.60
_diffrn_reflns_theta_max         25.60
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0857P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1789
_reflns_number_gt                3223
_reflns_number_total             6333
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3072.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2016509
_cod_database_fobs_code          2016509