A Robust Open Framework Formed by Decavanadate Clusters and Copper(II) Complexes of Macrocyclic Polyamines: Permanent Microporosity and Catalytic Oxidation of Cycloalkanes.
Martín-Caballero, Jagoba; San José Wéry, Ana; Reinoso, Santiago; Artetxe, Beñat; San Felices, Leire; El Bakkali, Bouchra; Trautwein, Guido; Alcañiz-Monge, Juan; Vilas, José Luis; Gutiérrez-Zorrilla, Juan M; Inorganic chemistry 55 (2016) 4970–4979; doi:10.1021/acs.inorgchem.6b00505

data_4347707
_publ_section_title
;
 A Robust Open Framework Formed by Decavanadate Clusters and Copper(II)
 Complexes of Macrocyclic Polyamines: Permanent Microporosity and
 Catalytic Oxidation of Cycloalkanes.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4970
_journal_page_last               4979
_journal_paper_doi               10.1021/acs.inorgchem.6b00505
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C30 H92 Cu3 N12 O38 V10'
_chemical_formula_sum            'C30 H92 Cu3 N12 O38 V10'
_chemical_formula_weight         1929.18
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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_audit_creation_date             2015-12-21T17:07:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                95.752(5)
_cell_angle_beta                 105.003(6)
_cell_angle_gamma                90.677(6)
_cell_formula_units_Z            1
_cell_length_a                   10.6665(8)
_cell_length_b                   11.9325(9)
_cell_length_c                   13.7832(8)
_cell_measurement_reflns_used    4055
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.704
_cell_measurement_theta_min      3.305
_cell_volume                     1684.7(2)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
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_computing_data_reduction
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'OLEX2 (Dolomanov, 2009)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2012
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0990346
_diffrn_orient_matrix_UB_12      -0.0947405
_diffrn_orient_matrix_UB_13      0.0007099
_diffrn_orient_matrix_UB_21      0.1054576
_diffrn_orient_matrix_UB_22      -0.0874188
_diffrn_orient_matrix_UB_23      0.0016136
_diffrn_orient_matrix_UB_31      0.038262
_diffrn_orient_matrix_UB_32      0.0156768
_diffrn_orient_matrix_UB_33      0.1163691
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11577
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    12.928
_exptl_absorpt_correction_T_max  0.701
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
        (compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             977
_exptl_crystal_size_max          0.1566
_exptl_crystal_size_mid          0.0755
_exptl_crystal_size_min          0.0371
_refine_diff_density_max         2.145
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         5977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.07
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0965P)^2^+2.3804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1661
_reflns_number_gt                4821
_reflns_number_total             5977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00505_si_002.cif
_cod_data_source_block           1
_cod_database_code               4347707