Alcoholysis of 2,2'-Pyridil, (2-C5H4N)C(O)C(O)(2-C5H4N), in the Presence of Copper(II): A Family of Planar Pentanuclear Copper(II) Complexes Stabilized by [(2-C5H4N)C(O)(OR)C(O)(OR)(2-C5H4N)]2- and Carboxylate Ligands
Giannis S. Papaefstathiou; Catherine P. Raptopoulou; Alexandros Tsohos; Aris Terzis; Evangelos G. Bakalbassis; Spyros P. Perlepes; Inorganic Chemistry 39 (2000) 4658–4662; doi:10.1021/ic991169k

data_4321419
_publ_section_title
;
 Alcoholysis of 2,2'-Pyridil, (2-C5H4N)C(O)C(O)(2-C5H4N), in the Presence
 of Copper(II): A Family of Planar Pentanuclear Copper(II) Complexes
 Stabilized by [(2-C5H4N)C(O)(OR)C(O)(OR)(2-C5H4N)]2- and Carboxylate
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4658
_journal_page_last               4662
_journal_paper_doi               10.1021/ic991169k
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C48 H74 Cu5 N4 O22'
_chemical_formula_weight         1376.81
_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                65.433(4)
_cell_angle_beta                 81.488(4)
_cell_angle_gamma                74.338(3)
_cell_formula_units_Z            1
_cell_length_a                   12.522(1)
_cell_length_b                   11.117(1)
_cell_length_c                   12.643(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      27
_cell_measurement_theta_min      11
_cell_volume                     1540.0(2)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic package, C.E.Strouse, 1994)'
_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
'P21 Nicolet diffractometer upgraded by Crystal Logic'
_diffrn_measurement_method       'theta-2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5464
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         5.21
_diffrn_standards_decay_%        2.8
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.539
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_meas      1.46
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             711
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.041
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         5207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_restrained_S_obs      1.041
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_obs          0.0381
_refine_ls_shift/esd_max         -1.295
_refine_ls_shift/esd_mean        0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+1.1669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1115
_refine_ls_wR_factor_obs         0.1011
_reflns_number_observed          4350
_reflns_number_total             5207
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991169k_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^)+(0.0504P)^2^+1.1669P] 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^)+(0.0504P)^2^+1.1669P] 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        1539.9(3)
_cod_database_code               4321419