Syntheses, Crystal Structures, and Magnetic Properties of One-Dimensional Oxalato-Bridged Co(II), Ni(II), and Cu(II) Complexes withn-Aminopyridine (n= 2-4) as Terminal Ligand
Oscar Castillo; Antonio Luque; Pascual Román; Francesc Lloret; Miguel Julve; Inorganic Chemistry 40 (2001) 5526–5535; doi:10.1021/ic0103401

data_4320386
_publ_contact_author
;
Antonio Luque. Departamento de Quimica Inorganica. Facultad de Ciencias
Universidad del Pais Vasco,  Apdo. 644, E-48080 Bilbao, Spain
;
_publ_contact_author_email       qipluara@lg.ehu.es
_publ_contact_author_fax         '+34-94-464 85 00'
_publ_contact_author_phone       '+34-946 012 701'
_publ_section_title
;
 Syntheses, Crystal Structures, and Magnetic Properties of One-Dimensional
 Oxalato-Bridged Co(II), Ni(II), and Cu(II) Complexes withn-Aminopyridine
 (n= 2-4) as Terminal Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5526
_journal_page_last               5535
_journal_paper_doi               10.1021/ic0103401
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'aqueous synthesis'
_chemical_formula_structural     '[Cu(C2O4)(C5H6N2)2].1.5H20'
_chemical_formula_sum            'C12 H15 Cu N4 O5.5'
_chemical_formula_weight         366.82
_chemical_name_systematic
;
catena-(mu-oxalato)-bis(3-aminopyridine)-copper(II)-water (1/1.5)
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2c'
_symmetry_space_group_name_H-M   'P c n n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             12-mar-01
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.387(1)
_cell_length_b                   12.935(3)
_cell_length_c                   18.632(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.52
_cell_measurement_theta_min      3.30
_cell_volume                     2985.3(8)
_computing_cell_refinement       'local programs'
_computing_data_collection       ' CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'DIRDIF-92 (Beurskens, 1992)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD4 diffractometer'
_diffrn_measurement_method       '\w/2\q mode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4838
_diffrn_reflns_theta_max         29.95
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.58
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_meas      1.62(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.464
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_all   1.216
_refine_ls_goodness_of_fit_gt    1.303
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.216
_refine_ls_restrained_S_gt       1.303
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/esd_mean        0.010
_refine_ls_shift/su_max          0.075
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1968
_refine_ls_wR_factor_gt          0.1930
_reflns_number_gt                3670
_reflns_number_total             4343
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic0103401_4.cif
_cod_data_source_block           compound6
_cod_original_formula_sum        'C12 H15 Cu1 N4 O5.5'
_cod_database_code               4320386