Dicopper(II) Metallacyclophanes with N,N'-2,6-Pyridinebis(oxamate): Solution Study, Synthesis, Crystal Structures, and Magnetic Properties.
Fernandes, Tamires S.; Vilela, Ramon S.; Valdo, Ana K.; Martins, Felipe T.; García-España, Enrique; Inclán, Mario; Cano, Joan; Lloret, Francesc; Julve, Miguel; Stumpf, Humberto O.; Cangussu, Danielle; Inorganic chemistry 55 (2016) 2390–2401; doi:10.1021/acs.inorgchem.5b02786

data_4347137
_publ_section_title
;
 Dicopper(II) Metallacyclophanes with N,N'-2,6-Pyridinebis(oxamate):
 Solution Study, Synthesis, Crystal Structures, and Magnetic Properties.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2390
_journal_page_last               2401
_journal_paper_doi               10.1021/acs.inorgchem.5b02786
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C26 H38.4 Cu2 K N8 Na O16.2'
_chemical_formula_weight         911.44
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m c e'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.521(18)
_cell_length_b                   13.220(18)
_cell_length_c                   24.87(3)
_cell_measurement_reflns_used    9766
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      1.96
_cell_volume                     7404(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9766
_diffrn_reflns_theta_full        25.62
_diffrn_reflns_theta_max         25.62
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    1.354
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R. H. (1995) Acta Cryst., A51, 33-38'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+1.2921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1306
_reflns_number_gt                2473
_reflns_number_total             3534
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5b02786_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        7406(14)
_cod_original_sg_symbol_H-M      Cmca
_cod_original_formula_sum        'C26 H38.40 Cu2 K N8 Na O16.20'
_cod_database_code               4347137