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_4335681
_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         'C64 H78 Cu2 N12 Na2 O8'
_chemical_formula_sum            'C64 H78 Cu2 N12 Na2 O8'
_chemical_formula_weight         1316.47
_chemical_name_common            LCu(OTHF)Na
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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            4
_cell_length_a                   14.131(4)
_cell_length_b                   16.013(5)
_cell_length_c                   32.378(10)
_cell_measurement_reflns_used    10215
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      1.79
_cell_volume                     7326(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1767
_diffrn_reflns_av_sigmaI/netI    0.2276
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            32342
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.9808
_exptl_absorpt_correction_T_min  0.9621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_meas      1.193
_exptl_crystal_description       Block
_exptl_crystal_F_000             2759
_exptl_crystal_recrystallization_method
'Et2O diffused slowly into the MeCN solution at -20 \%C '
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10215
_refine_ls_number_restraints     827
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.1657
_refine_ls_R_factor_gt           0.0916
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0992P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1953
_refine_ls_wR_factor_ref         0.2277
_reflns_number_gt                4748
_reflns_number_total             10215
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401446s_si_003_2.cif
_cod_data_source_block           4
_cod_database_code               4335681