Reversible conversion of valence-tautomeric copper metal-organic frameworks dependent single-crystal-to-single-crystal oxidation/reduction: a redox-switchable catalyst for C-H bonds activation reaction
Chao Huang; Jie Wu; Chuanjun Song; Ran Ding; Yan Qiao; Hongwei Hou; Junbiao Chang; Yaoting Fan; Chem.Commun. 51 (2015) 10353–; doi:10.1039/C5cc02432C

data_7117298
_publ_section_title
;
 Reversible conversion of valence-tautomeric copper metal-organic
 frameworks dependent single-crystal-to-single-crystal
 oxidation/reduction: a redox-switchable catalyst for C-H bonds activation
 reaction
;
_journal_name_full               Chem.Commun.
_journal_page_first              10353
_journal_paper_doi               10.1039/C5cc02432C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C6 H4 Cu2 N9 O1.50'
_chemical_formula_sum            'C6 H4 Cu2 N9 O1.5'
_chemical_formula_weight         353.26
_chemical_name_systematic        'Cu(I)Cu(II) complex'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-01-03 deposited with the CCDC.
2015-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 119.89(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.338(5)
_cell_length_b                   9.4877(19)
_cell_length_c                   16.502(3)
_cell_measurement_reflns_used    4576
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8884
_cell_measurement_theta_min      2.3497
_cell_volume                     3303.6(15)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Saturn724
_diffrn_measurement_method       dtprofit.ref
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3066
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         4240
_exptl_absorpt_coefficient_mu    2.581
_exptl_absorpt_correction_T_max  0.6829
_exptl_absorpt_correction_T_min  0.6133
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC Inc., 2006)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
The unit cell includes a large region of disordered solvent water molecules,
which could not be modeled as discrete atomic sites. We employed PLATON/SQUEEZE 
to calculate the diffraction contribution of the solvent water molecules and, 
thereby, to produce a set of solvent-free diffraction intensities.Combing  
single-crystal structures, elemental microanalyses, TGA and the electron count 
of the SQUEEZE results, about 1.5 water molecules per asymmetric unit
;
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3066
_refine_ls_number_restraints     227
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0882P)^2^+11.7132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1572
_reflns_number_gt                2745
_reflns_number_total             3066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc02432c2.cif
_cod_data_source_block           b
_cod_original_cell_volume        3303.7(11)
_cod_original_sg_symbol_Hall     '-C 2yc  '
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_original_formula_sum        'C6 H4 Cu2 N9 O1.50'
_cod_database_code               7117298