Synthesis and structure of a Cu4O4 cubane core complex from a carboxylate ligand containing a strong pi pi stacking supramolecular synthon
Daniel L. Reger; Agota Debreczeni; Mark D. Smith; Inorganica Chimica Acta 386 (2012) 102–108; doi:10.1016/j.ica.2012.01.041

data_1513076
_publ_section_title
;
 Synthesis and structure of a Cu4O4 cubane core complex from a carboxylate
 ligand containing a strong pi pi stacking supramolecular synthon
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              102
_journal_page_last               108
_journal_paper_doi               10.1016/j.ica.2012.01.041
_journal_volume                  386
_journal_year                    2012
_chemical_formula_moiety         'C81 H74 Cu4 N6 O21'
_chemical_formula_sum            'C81 H74 Cu4 N6 O21'
_chemical_formula_weight         1721.62
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 115.139(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.108(4)
_cell_length_b                   27.934(4)
_cell_length_c                   28.988(4)
_cell_measurement_reflns_used    5229
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      22.218
_cell_measurement_theta_min      2.165
_cell_volume                     20605(5)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    various
_computing_publication_material  'SHELXTL Version 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_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  0.0727
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            85945
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             7088
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         10792
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0962P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                6856
_reflns_number_total             10792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ad07.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1513076