Oxidative Cyclization of 1,5-Dienes with Hydrogen Peroxide Catalyzed by an Osmium(III) Complex: Synthesis of cis-Tetrahydrofurans.
Sugimoto, Hideki; Kanetake, Takayuki; Maeda, Kazuki; Itoh, Shinobu; Organic letters 18 (2016) 1246–1249; doi:10.1021/acs.orglett.6b00064

data_1542736
_publ_section_title
;
 Oxidative Cyclization of 1,5-Dienes with Hydrogen Peroxide Catalyzed by
 an Osmium(III) Complex: Synthesis of cis-Tetrahydrofurans.
;
_journal_issue                   6
_journal_name_full               'Organic letters'
_journal_page_first              1246
_journal_page_last               1249
_journal_paper_doi               10.1021/acs.orglett.6b00064
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C20 H19 N4 O2 Os, 2(C F3 O3 S)'
_chemical_formula_sum            'C22 H19 F6 N4 O8 Os S2'
_chemical_formula_weight         835.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.2030
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   14.8667
_cell_length_b                   23.2445
_cell_length_c                   16.5946
_cell_measurement_reflns_used    27161
_cell_measurement_temperature    103
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.02
_cell_volume                     5733.315
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      103
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1361
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54734
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.017
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.682
_exptl_absorpt_correction_T_max  0.626
_exptl_absorpt_correction_T_min  0.126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.936
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unknown
_exptl_crystal_F_000             3240.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         5.080
_refine_diff_density_min         -5.930
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     809
_refine_ls_number_reflns         13100
_refine_ls_R_factor_gt           0.0777
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1876
_reflns_number_gt                7263
_reflns_number_total             13100
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol6b00064_si_002.cif
_cod_data_source_block           20141218
_cod_depositor_comments
;
          Adding full bibliography for 1542736.cif.

2019-02-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C44 H38 F12 N8 O16 Os2 S4'
_cod_original_formula_weight         1671.45
_cod_original_formula_moiety         'C44 H38 F12 N8 O16 Os2 S4'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        5733.3129
_cod_database_code               1542736