Molecular-Programmed Self-Assembly of Homo- and Heterometallic Penta- and Hexanuclear Coordination Compounds: Synthesis, Crystal Structures, and Magnetic Properties of Ladder-Type CuII2MIIx (M = Cu, Ni;x= 3, 4) Oxamato Complexes with CuII2 Metallacyclophane Cores
Emilio Pardo; Rafael Ruiz-García; Francesc Lloret; Miguel Julve; Joan Cano; Jorge Pasán; Catalina Ruiz-Pérez; Yasmine Filali; Lise-Marie Chamoreau; Yves Journaux; Inorganic Chemistry 46 (2007) 4504–4514; doi:10.1021/ic062453w

data_4307961
_publ_contact_author_address
;
 Laboratorio de Rayos X y Materiales Moleculares
 Dpto. F\'isica Fundamental II. Facultad de F\'isica
 Universidad de La Laguna
 E-38204. La Laguna. Tenerife
 Spain
;
_publ_contact_author_email       caruiz@ull.es
_publ_contact_author_name        'Professor Catalina Ruiz-P\'erez'
_publ_section_title
;
Molecular-Programmed Self-Assembly of Homo- and Heterometallic Penta- and
Hexanuclear Coordination Compounds: Synthesis, Crystal Structures, and
Magnetic Properties of Ladder-Type CuII2MIIx (M = Cu, Ni;x= 3, 4) Oxamato
Complexes with CuII2 Metallacyclophane Cores
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4504
_journal_page_last               4514
_journal_paper_doi               10.1021/ic062453w
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C56 H112 Cu6 F19 N16 O18 P3'
_chemical_formula_weight         2132.77
_chemical_name_systematic
;
 ?
;
_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-97
_cell_angle_alpha                88.69(4)
_cell_angle_beta                 78.06(3)
_cell_angle_gamma                77.72(2)
_cell_formula_units_Z            2
_cell_length_a                   14.821(3)
_cell_length_b                   17.246(7)
_cell_length_c                   19.253(9)
_cell_measurement_temperature    293(2)
_cell_volume                     4703(3)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    CRYSTALMAKER
_computing_publication_material  'PARST97 (Nardelli, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1032
_diffrn_reflns_av_sigmaI/netI    0.1692
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36002
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         6.41
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.483
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             2162
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.366
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1066
_refine_ls_number_reflns         15217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1991
_refine_ls_R_factor_gt           0.0968
_refine_ls_shift/su_max          0.866
_refine_ls_shift/su_mean         0.495
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1808P)^2^+5.7728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1864
_refine_ls_wR_factor_ref         0.3229
_reflns_number_gt                7141
_reflns_number_total             15217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062453w-file003.cif
_cod_data_source_block           compound-3
_cod_database_code               4307961