The Goldilocks principle in action: synthesis and structural characterization of a novel {Cu4(μ3-OH)4} cubane stabilized by monodentate ligands.
Ardizzoia, G. Attilio; Brenna, Stefano; Durini, Sara; Therrien, Bruno; Trentin, Ivan; Dalton transactions (Cambridge, England : 2003) 42 (2013) 12265–12273; doi:10.1039/c3dt51017d

data_7023216
_publ_section_title
;
 The Goldilocks principle in action: synthesis and structural
 characterization of a novel {Cu4(\m3-OH)4} cubane stabilized by
 monodentate ligands.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12265
_journal_page_last               12273
_journal_paper_doi               10.1039/c3dt51017d
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C48 H84 Cu4 N16 O4, 4 (Cl O4)'
_chemical_formula_sum            'C48 H84 Cl4 Cu4 N16 O20'
_chemical_formula_weight         1601.27
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 122.694(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9451(6)
_cell_length_b                   30.6995(8)
_cell_length_c                   20.6734(9)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      1.48
_cell_volume                     8516.5(6)
_computing_cell_refinement       'CELL (Stoe & Cie, 2000)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 2000)'
_computing_molecular_graphics    'ORTEP-32 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'phi oscillation'
_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  0.1237
_diffrn_reflns_av_unetI/netI     0.1306
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            109282
_diffrn_reflns_theta_full        29.35
_diffrn_reflns_theta_max         29.35
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
Upon examination of the crystal packing of complex 3 with PLATON
(Spek, 2003), two large solvent accessible voids were observed. 
These solvent accessible voids occupy an area of 
approximately 1240 \%A^3^. Chemical evidence suggests that 
diethylether molecules sit in these regions, however, 
the electron densities in these areas are quite low and 
it was not possible to define crystallographically the 
solvent molecules. Therefore, a data set corresponding to 
omission of the missing solvent was generated using the SQUEEZE
(Spek, 2003; van der Sluis & Spek, 1990) 
algorithm from PLATON and the structure was refined to convergence.
;
_refine_diff_density_max         1.737
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         23126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1880
_refine_ls_R_factor_gt           0.1020
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0959P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.2306
_reflns_number_gt                13196
_reflns_number_total             23126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51017d.txt
_cod_data_source_block           d:complex3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        8516.5(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7023216