Isolation of a 2-Hydroxytetrahydrofuran Complex from Copper-Promoted Hydroxylation of THF
Mohammad Reza Halvagar; William B. Tolman; Inorganic Chemistry 52 (2013) 8306–8308; doi:10.1021/ic401446s

data_4335680
_publ_contact_author_email       wtolman@umn.edu
_publ_contact_author_name        'William B. Tolman'
_publ_section_title
;
 Isolation of a 2-Hydroxytetrahydrofuran Complex from Copper-Promoted
 Hydroxylation of THF
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8306
_journal_page_last               8308
_journal_paper_doi               10.1021/ic401446s
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C56 H66 Cu2 N12 Na2 O6'
_chemical_formula_sum            'C56 H66 Cu2 N12 Na2 O6'
_chemical_formula_weight         1176.29
_chemical_name_common            LCu(OH)Na
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      130
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.702(4)
_cell_length_b                   27.702(4)
_cell_length_c                   14.175(2)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.08
_cell_volume                     10878(3)
_computing_cell_refinement       'SMART, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SMART, Bruker'
_computing_publication_material  'SMART, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART Platform, CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            88130
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.861
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            'pale purple'
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       Block
_exptl_crystal_F_000             4911
_exptl_crystal_recrystallization_method 'slow evaporation from THF solution'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.00007(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4793
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+27.9681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                3249
_reflns_number_total             4793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401446s_si_003_1.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4335680