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_7025296
_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            'C84 H150 Cl6 Cu6 N24 Na2 Ni2 O54'
_chemical_formula_weight         3119.58
_chemical_name_systematic
;
?
;
_space_group_IT_number           188
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c 2'
_symmetry_space_group_name_H-M   'P -6 c 2'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   17.426(3)
_cell_length_b                   17.426(3)
_cell_length_c                   31.674(6)
_cell_measurement_temperature    293(2)
_cell_volume                     8330(3)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'MxCube (ESRF, 2006)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_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 9.6
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_detector       'ADSC Q210r CCD (binned mode)'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_wavelength     0.72930
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            72097
_diffrn_reflns_theta_full        23.93
_diffrn_reflns_theta_max         23.93
_diffrn_reflns_theta_min         1.91
_diffrn_source                   synchrotron
_diffrn_source_type              'ESRF-CRG BM16'
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prisms'
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.896
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4112
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0970
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2465
_refine_ls_wR_factor_ref         0.2504
_reflns_number_gt                3833
_reflns_number_total             4112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b926709c.txt
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        8330(2)
_cod_original_sg_symbol_H-M      P-6c2
_cod_database_code               7025296