Aerial oxidation of tetrahydrofuran to 2-hydroxotetrahydrofuran in the presence of a trimeric CuI complex [Cu3L3] (HL = tBuNHC(S)NHP(S)(OiPr)2) and trapping of the unstable product at recrystallization
Luckay, Robert C.; Sheng, Xia; Strasser, Christoph E.; Raubenheimer, Helgard G.; Safin, Damir A.; Babashkina, Maria G.; Klein, Axel; New Journal of Chemistry 34 (2010) 2835–; doi:10.1039/c0nj00314j

data_7053630
_publ_section_title
;
 Aerial oxidation of tetrahydrofuran to 2-hydroxotetrahydrofuran in the
 presence of a trimeric CuI complex [Cu3L3] (HL = tBuNHC(S)NHP(S)(OiPr)2)
 and trapping of the unstable product at recrystallization
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2835
_journal_paper_doi               10.1039/c0nj00314j
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C33 H72 Cu3 N6 O6 P3 S6, C4 H8 O2'
_chemical_formula_sum            'C37 H80 Cu3 N6 O8 P3 S6'
_chemical_formula_weight         1213.05
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.100(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.448(7)
_cell_length_b                   15.407(7)
_cell_length_c                   25.575(11)
_cell_measurement_reflns_used    31783
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      1.9
_cell_volume                     5692(5)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART Apex CCD diffractometer'
_diffrn_measurement_method       \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  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            32467
_diffrn_reflns_theta_full        26.55
_diffrn_reflns_theta_max         26.55
_diffrn_reflns_theta_min         1.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.462
_exptl_absorpt_correction_T_max  0.7362
_exptl_absorpt_correction_T_min  0.6615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.332
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         11760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+13.2054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                9428
_reflns_number_total             11760
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c0nj00314j.txt
_cod_data_source_block           Safin1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        5692(4)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7053630