Three New Polynuclear Copper(II) Complexes with the Symmetric [Cu(μ1,1-N3)2Cu]2+ Core and Pyridine Derivatives: Syntheses, Structure, and Magnetic Behavior
Albert Escuer; Mohamed A. S. Goher; Franz A. Mautner; Ramon Vicente; Inorganic Chemistry 39 (2000) 2107–2112; doi:10.1021/ic991135c

data_4320928
_publ_section_title
;
 Three New Polynuclear Copper(II) Complexes with the Symmetric
 [Cu(\m1,1-N3)2Cu]2+ Core and Pyridine Derivatives: Syntheses, Structure,
 and Magnetic Behavior
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2107
_journal_page_last               2112
_journal_paper_doi               10.1021/ic991135c
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C20 H28 Cu3 N22 O6'
_chemical_formula_weight         863.26
_chemical_name_common            '[Cu3(N3)6(Methyl-Isonicotinate)2(DMF)2]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.81(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.755(2)
_cell_length_b                   14.680(5)
_cell_length_c                   15.810(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      7.0
_cell_volume                     1755.1(9)
_computing_molecular_graphics    'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)'
_computing_publication_material  'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'mod. STOE 4-circle diffractometer'
_diffrn_measurement_method       'Omega-Scan; delta Omega: 1.25 deg.'
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0809
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4361
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  '1 h'
_diffrn_standards_number         '3 (1 1 4, -1 -2 -1, 2 2 -2)'
_exptl_absorpt_coefficient_mu    1.870
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_meas      1.61(3)
_exptl_crystal_density_method    'suspension method'
_exptl_crystal_description       prism
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   0.986
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_restrained_S_obs      0.986
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_obs          0.0481
_refine_ls_shift/esd_max         -0.047
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1276
_refine_ls_wR_factor_obs         0.1073
_reflns_number_observed          2270
_reflns_number_total             3625
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991135c_3.cif
_cod_data_source_block           gh31
_cod_depositor_comments
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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 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0746P)^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^)+(0.0746P)^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 
;
_cod_database_code               4320928