A Cu(ii) MOF with a flexible bifunctionalised terpyridine as an efficient catalyst for the single-pot hydrocarboxylation of cyclohexane to carboxylic acid in water/ionic liquid medium.
Paul, Anup; Ribeiro, Ana P. C.; Karmakar, Anirban; Guedes da Silva, M Fátima C; Pombeiro, Armando J. L.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12779–12789; doi:10.1039/c6dt01852a

data_7039926
_publ_section_title
;
 A Cu(ii) MOF with a flexible bifunctionalised terpyridine as an efficient
 catalyst for the single-pot hydrocarboxylation of cyclohexane to
 carboxylic acid in water/ionic liquid medium.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12779
_journal_page_last               12789
_journal_paper_doi               10.1039/c6dt01852a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C29 H20 Cu N4 O6, (C3 H7 N O)'
_chemical_formula_sum            'C32 H27 Cu N5 O7'
_chemical_formula_weight         657.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-05-11 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 123.341(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.819(6)
_cell_length_b                   8.5131(15)
_cell_length_c                   22.168(4)
_cell_measurement_reflns_used    5272
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.51
_cell_measurement_theta_min      2.48
_cell_volume                     5804.8(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury CSD 3.5.1, 2008'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1999)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1980
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61720
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.507
_diffrn_reflns_theta_min         2.334
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       Block
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.210
_platon_squeeze_details
;
 The Platon SQUEEZE procedure was applied to recover 308 electrons per
 unit cell in a void (total volume 996 A^3), that is, 38 electrons
 per formula unit. On the basis of microanalytical data, the void content
 may include 1 dmf molecule per unit cell, i.e., a total of 320 electrons
 not far from the values estimated by SQUEEZE.  
 PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.861
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5987
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0828
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1828P)^2^+32.9749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2238
_refine_ls_wR_factor_ref         0.2825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3332
_reflns_number_total             5987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01852a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7039926.cif.'
_cod_database_code               7039926
_shelx_estimated_absorpt_t_min   0.787
_shelx_estimated_absorpt_t_max   0.848
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              37827
_shelx_fab_checksum              50886