A tetragonal Bisphenoidal Tetracopper(I) Arrangement Supported by a Potentially Tridentate Ligand Containing Thiolate, Secondary Amine, and 2-Pyridine Functions: Hydrogen-Bonded Instead of Cu(I)-Coordinated Pyridine Rings in an S4-Symmetric Compound
Andreas F. Stange; Karl Wilhelm Klinkhammer; Wolfgang Kaim; Inorganic Chemistry 35 (1996) 4087–4089; doi:10.1021/ic951629j

data_4323852
_publ_contact_author
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        Prof. Dr. W. Kaim
        Institut f\"ur Anorganische Chemie
        Universit\"at Stuttgart
        Pfaffenwaldring 55
        70550 Stuttgart
        Bundesrepublik Deutschland
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_publ_contact_author_email       ak-kaim@rus.uni-stuttgart.de
_publ_contact_author_fax         '049 711 685-4241'
_publ_contact_author_phone       '049 711 685-4171'
_publ_section_title
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 A tetragonal Bisphenoidal Tetracopper(I) Arrangement Supported by a
 Potentially Tridentate Ligand Containing Thiolate, Secondary Amine, and
 2-Pyridine Functions: Hydrogen-Bonded Instead of Cu(I)-Coordinated
 Pyridine Rings in an S4-Symmetric Compound
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4087
_journal_page_last               4089
_journal_paper_doi               10.1021/ic951629j
_journal_volume                  35
_journal_year                    1996
_chemical_formula_analytical     'C32 H44 Cu4 N8 S4'
_chemical_formula_moiety         'C32 H44 Cu4 N8 S4'
_chemical_formula_structural     'C32 H44 Cu4 N8 S4'
_chemical_formula_sum            'C32 H44 Cu4 N8 S4'
_chemical_formula_weight         923.15
_chemical_name_common            Cu4(MEPA)4
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.556(2)
_cell_length_b                   12.556(2)
_cell_length_c                   11.826(2)
_cell_measurement_reflns_used    65
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      25
_cell_volume                     1864.4(5)
_computing_cell_refinement       'Siemens Diffractometer Software'
_computing_data_collection       'Siemens Diffractometer Software'
_computing_data_reduction        'SHELXTL-Plus XDISK'
_computing_molecular_graphics    'SHELXTL-PLUS XP'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4347
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    2.510
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.030
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_restrained_S_obs      1.030
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_obs          0.0367
_refine_ls_shift/esd_max         -0.018
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0953
_refine_ls_wR_factor_obs         0.0931
_reflns_number_observed          2090
_reflns_number_total             2169
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic951629j.cif
_cod_data_source_block           i4
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.0000P] 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^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323852