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_4307962
_publ_contact_author
;
Yves Journaux
;
_publ_contact_author_email       jour@ccr.jussieu.fr
_publ_contact_author_fax         '00 33 1 44 27 '
_publ_contact_author_phone       '00 33 1 44 27 '
_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_moiety
'(C62 H112 Cu6 N16 O12)4+,4 (ClO4)-, 14(H2O) '
_chemical_formula_sum            'C62 H140 Cl4 Cu6 N16 O42'
_chemical_formula_weight         2304.94
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.013(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.580(5)
_cell_length_b                   16.392(2)
_cell_length_c                   31.014(4)
_cell_measurement_reflns_used    238
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      20.6
_cell_measurement_theta_min      3.4
_cell_volume                     10105(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    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.1017
_diffrn_reflns_av_sigmaI/netI    0.1465
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            101510
_diffrn_reflns_theta_full        29.4
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4808
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1150
_refine_ls_number_reflns         29276
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1994
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1137P)^2^+29.8766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2287
_refine_ls_wR_factor_ref         0.2718
_reflns_number_gt                13448
_reflns_number_total             29276
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062453w-file004.cif
_cod_data_source_block           yf396
_cod_original_cell_volume        10106(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4307962