Copper-promoted aerial oxidation of benzothiadiazines: access to benzothiadiazine S-oxide heterocycles.
Clark, Ewan R.; Hayward, John J.; Leontowicz, Bryce J.; Anwar, Muhammad U.; Pilkington, Melanie; Rawson, Jeremy M.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 2071–2074; doi:10.1039/c4dt03467h

data_7033401
_publ_section_title
;
 Copper-promoted aerial oxidation of benzothiadiazines: access to
 benzothiadiazine S-oxide heterocycles.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2071
_journal_page_last               2074
_journal_paper_doi               10.1039/c4dt03467h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C48 H32 Cu2 N12 O4 S4, 2(C H4 O) '
_chemical_formula_sum            'C50 H40 Cu2 N12 O6 S4'
_chemical_formula_weight         1160.26
_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
_audit_update_record
;
2014-12-09 deposited with the CCDC.
2014-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                75.65(3)
_cell_angle_beta                 88.65(3)
_cell_angle_gamma                68.44(3)
_cell_formula_units_Z            1
_cell_length_a                   8.9974(18)
_cell_length_b                   10.434(2)
_cell_length_c                   14.204(3)
_cell_measurement_reflns_used    9580
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     1198.1(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics    'Mercury v.3.0 (CCD), XP'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11353
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

multi-scan from symmetry-related measurements
 
 Sortav (Blessing 1995)

;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         3124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+1.6368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                2621
_reflns_number_total             3124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03467h2.cif
_cod_data_source_block           complex_4
_cod_depositor_comments
'Adding full bibliography for 7033401--7033404.cif.'
_cod_original_cell_volume        1198.1(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7033401