Modulating the packing of [Cu24(isophthalate)24] cuboctahedra in a triazole-containing metal‒organic polyhedral framework
Yan, Yong; Suyetin, Mikhail; Bichoutskaia, Elena; Blake, Alexander J.; Allan, David R.; Barnett, Sarah A.; Schröder, Martin; Chemical Science 4 (2013) 1731–; doi:10.1039/c3sc21769h

data_1514430
_publ_section_title
;
 Modulating the packing of [Cu24(isophthalate)24] cuboctahedra in a
 triazole-containing metal--organic polyhedral framework
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1731
_journal_paper_doi               10.1039/c3sc21769h
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'Cu3 C36 H21 N9 O15, 10(C3 H7 N O), 10(H2 O)'
_chemical_formula_sum            'C66 H111 Cu3 N19 O35'
_chemical_formula_weight         1921.36
_chemical_name_systematic
;
?
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   30.926(5)
_cell_length_b                   30.926(5)
_cell_length_c                   45.103(7)
_cell_measurement_reflns_used    56775
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.7
_cell_measurement_theta_min      0.9
_cell_volume                     43137(12)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond Beamline I19'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.064
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            53063
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         0.88
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       'truncated octahedron'
_exptl_crystal_F_000             16112
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Approximately 74% of the unit cell volume comprises a large region of
disordered solvent which could not be modelled as discrete atomic sites.
We employed PLATON SQUEEZE to calculate the contribution to the diffraction
from the solvent region. SQUEEZE estimated a total count of 6889 electrons
per unit cell, and thereby produced a set of solvent-free diffraction
intensities. The final formula was calculated from the TGA results combined
with elemental analysis data.
;
_refine_diff_density_max         1.18
_refine_diff_density_min         -0.55
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         18798
_refine_ls_number_restraints     488
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0649
_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^)+(0.126P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.189
_refine_ls_wR_factor_ref         0.201
_reflns_number_gt                13280
_reflns_number_total             18798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc21769h.txt
_cod_data_source_block           yyculg
_cod_original_cell_volume        43137(11)
_cod_database_code               1514430