Octanuclearity in Copper(II) Chemistry: Preparation, Characterization, and Magnetochemistry of [Cu8(dpk.OH)8(O2CCH3)4](ClO4)4.9H2O (dpk.H2O = the Hydrated, gem-Diol Form of Di-2-pyridyl Ketone)
Vasilis Tangoulis; Catherine P. Raptopoulou; Aris Terzis; Sofia Paschalidou; Spyros P. Perlepes; Evangelos G. Bakalbassis; Inorganic Chemistry 36 (1997) 3996–4006; doi:10.1021/ic961137m

data_4323553
_publ_section_title
;
 Octanuclearity in Copper(II) Chemistry: Preparation, Characterization,
 and Magnetochemistry of [Cu8(dpk.OH)8(O2CCH3)4](ClO4)4.9H2O (dpk.H2O =
 the Hydrated, gem-Diol Form of Di-2-pyridyl Ketone)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3996
_journal_page_last               4006
_journal_paper_doi               10.1021/ic961137m
_journal_volume                  36
_journal_year                    1997
_chemical_formula_analytical     '[Cu(C11 H10 N2 O2)2](C2 H3 O2)(ClO4).2H2O'
_chemical_formula_structural     '[Cu(dpk.H2O)2](O2CMe)(ClO4).2H2O'
_chemical_formula_sum            'C24 H27 Cl Cu N4 O12'
_chemical_formula_weight         662.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.19(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.000(2)
_cell_length_b                   8.008(1)
_cell_length_c                   27.095(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      5.5
_cell_volume                     2816.3(6)
_computing_cell_refinement       'Program LEAST, Crystal Logic Software'
_computing_data_collection       'Program COLLECT, Crystal Logic Software'
_computing_data_reduction        'Program REDUCE, Crystal Logic Software'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device
'Crystal Logic Dual Goniometer diffractometer'
_diffrn_measurement_method       'theta-2theta scan'
_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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            5202
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  1.09
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_meas      1.50
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallepiped
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.007
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0090(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         4964
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.086
_refine_ls_restrained_S_obs      1.117
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_obs          0.0629
_refine_ls_shift/esd_max         1.520
_refine_ls_shift/esd_mean        0.044
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1033P)^2^+6.3329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1911
_refine_ls_wR_factor_obs         0.1721
_reflns_number_observed          3898
_reflns_number_total             4965
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961137m_2.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1033P)^2^+6.3329P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1033P)^2^+6.3329P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2816.4(6)
_cod_database_code               4323553