Synthesis and Synthetic Application of Chloro- and Bromofuroxans.
Matsubara, Ryosuke; Ando, Akihiro; Hasebe, Hayu; Kim, Hojin; Tsuneda, Takao; Hayashi, Masahiko; The Journal of organic chemistry 85 (2020) 5959–5972; doi:10.1021/acs.joc.0c00326

data_4038246
_publ_section_title
;
 Synthesis and Synthetic Application of Chloro- and Bromofuroxans.
;
_journal_issue                   9
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5959
_journal_page_last               5972
_journal_paper_doi               10.1021/acs.joc.0c00326
_journal_volume                  85
_journal_year                    2020
_chemical_formula_moiety         'C12 H13 Cl N2 O3'
_chemical_formula_sum            'C12 H13 Cl N2 O3'
_chemical_formula_weight         268.70
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.3519(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   7.5174(6)
_cell_length_b                   10.8721(9)
_cell_length_c                   7.6231(6)
_cell_measurement_reflns_used    2942
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.735
_cell_measurement_theta_min      2.712
_cell_volume                     622.51(9)
_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    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3491
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            NONE
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NONE
_exptl_crystal_F_000             280.00
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.220
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  755 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.49(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2190
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.0528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0612
_reflns_number_gt                2163
_reflns_number_total             2190
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo0c00326_si_003.cif
_cod_data_source_block           AA945_HPLC1_0am
_cod_depositor_comments
'Adding full bibliography for 4038245--4038253.cif.'
_cod_database_code               4038246