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_4323552
_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)
;
_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
'[Cu8(C11 H10 N2 O2)4(C2 H3 O2)4](ClO4)4.9H2O '
_chemical_formula_structural     '[Cu8(dpkOH)8(O2CMe)4](ClO4)4.9H2O'
_chemical_formula_sum            'C96 H102 Cl4 Cu8 N16 O49'
_chemical_formula_weight         2914.06
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                96.102(2)
_cell_angle_beta                 87.679(2)
_cell_angle_gamma                99.139(2)
_cell_formula_units_Z            2
_cell_length_a                   18.396(1)
_cell_length_b                   16.720(1)
_cell_length_c                   19.171(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      5.5
_cell_volume                     5787.1(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
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20914
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        2.8
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  1.26
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_meas      1.65
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallepiped
_exptl_crystal_F_000             2964
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.304
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.038
_refine_ls_goodness_of_fit_obs   1.066
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1486
_refine_ls_number_reflns         20237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_restrained_S_obs      1.066
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_obs          0.0550
_refine_ls_shift/esd_max         -0.585
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+14.0863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1763
_refine_ls_wR_factor_obs         0.1607
_reflns_number_observed          16184
_reflns_number_total             20239
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961137m_1.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^)+(0.0961P)^2^+14.0863P] 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^)+(0.0961P)^2^+14.0863P] 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        5786.9(7)
_cod_database_code               4323552