Variation of the ground spin state in homo- and hetero-octanuclear copper(ii) and nickel(ii) double-star complexes with a meso-helicate-type metallacryptand core
Pardo, Emilio; Dul, Marie-Claire; Lescouëzec, Rodrigue; Chamoreau, Lise-Marie; Journaux, Yves; Pasán, Jorge; Ruiz-Pérez, Catalina; Julve, Miguel; Lloret, Francesc; Ruiz-García, Rafael; Cano, Joan; Dalton Transactions 39 (2010) 4786–; doi:10.1039/b926709c

data_7025295
_publ_section_title
;
 Variation of the ground spin state in homo- and hetero-octanuclear
 copper(ii) and nickel(ii) double-star complexes with a meso-helicate-type
 metallacryptand core
;
_journal_issue                   20
_journal_name_full               'Dalton Transactions'
_journal_page_first              4786
_journal_paper_doi               10.1039/b926709c
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C22 H22 Cu N2 Na2 O9'
_chemical_formula_weight         567.93
_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                84.359(3)
_cell_angle_beta                 57.542(4)
_cell_angle_gamma                38.099(16)
_cell_formula_units_Z            4
_cell_length_a                   23.4405(15)
_cell_length_b                   19.8751(15)
_cell_length_c                   14.5335(15)
_cell_measurement_temperature    293(2)
_cell_volume                     2759(2)
_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    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_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 0.753
_diffrn_measured_fraction_theta_max 0.753
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.1239
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11917
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         6.40
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1164
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.814
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+1.8672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1427
_reflns_number_gt                4981
_reflns_number_total             9569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b926709c.txt
_cod_data_source_block           compound_Monomer
_cod_original_cell_volume        2759.1(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7025295