Selective Retention of Methanol over Ethanol by a Cyclen-Based Cryptand/Copper(II) Complex
Yoichi Habata; Mari Ikeda; Ajay K. Sah; Kanae Noto; Shunsuke Kuwahara; Inorganic Chemistry 52 (2013) 11697–11699; doi:10.1021/ic4021417

data_4336489
_publ_section_title
;
 Selective Retention of Methanol over Ethanol by a Cyclen-Based
 Cryptand/Copper(II) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11697
_journal_page_last               11699
_journal_paper_doi               10.1021/ic4021417
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C26 H34 N4 O5'
_chemical_formula_weight         482.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
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_symmetry_space_group_name_Hall  'C -2yc'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 118.076(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   39.522(4)
_cell_length_b                   12.4506(11)
_cell_length_c                   23.074(2)
_cell_measurement_reflns_used    4571
_cell_measurement_temperature    173
_cell_measurement_theta_max      22.06
_cell_measurement_theta_min      2.25
_cell_volume                     10018.0(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0400
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_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
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_diffrn_reflns_number            22561
_diffrn_reflns_theta_full        23.56
_diffrn_reflns_theta_max         23.56
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.9749
_exptl_absorpt_correction_T_min  0.9584
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1289
_refine_ls_number_reflns         11395
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0968P)^2^+11.2366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1687
_reflns_number_gt                9301
_reflns_number_total             11395
_reflns_threshold_expression     >2sigma(I)
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_cod_data_source_block           3
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