Synthesis of alkynyl furoxans. Rare carbon-carbon bond-forming reaction on a furoxan ring.
Matsubara, Ryosuke; Eguchi, Shuhei; Ando, Akihiro; Hayashi, Masahiko; Organic & biomolecular chemistry 15 (2017) 1965–1969; doi:10.1039/c7ob00181a

data_7155485
_publ_section_title
;
 Synthesis of alkynyl furoxans. Rare carbon-carbon bond-forming reaction
 on a furoxan ring.
;
_journal_issue                   9
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1965
_journal_page_last               1969
_journal_paper_doi               10.1039/c7ob00181a
_journal_volume                  15
_journal_year                    2017
_chemical_formula_moiety         'C18 H15 N5 O2'
_chemical_formula_sum            'C18 H15 N5 O2'
_chemical_formula_weight         333.35
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_update_record
;
2016-12-08 deposited with the CCDC.
2017-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.198(18)
_cell_formula_units_Z            8
_cell_length_a                   11.050(16)
_cell_length_b                   15.17(2)
_cell_length_c                   18.83(3)
_cell_measurement_reflns_used    255
_cell_measurement_temperature    90
_cell_measurement_theta_max      14.909
_cell_measurement_theta_min      2.163
_cell_volume                     3156(8)
_computing_cell_refinement       Unknown
_computing_data_collection       Unknown
_computing_data_reduction        Unknown
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.2018
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18368
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            NONE
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NONE
_exptl_crystal_F_000             1392.00
_exptl_crystal_size_max          0.000
_exptl_crystal_size_mid          0.000
_exptl_crystal_size_min          0.000
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.440
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     901
_refine_ls_number_reflns         13973
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.1137
_refine_ls_shift/su_max          0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0258P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2802
_reflns_number_gt                2680
_reflns_number_total             13994
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7ob00181a2.cif
_cod_data_source_block           SE_0ama
_cod_depositor_comments
'Adding full bibliography for 7155484--7155485.cif.'
_cod_database_code               7155485