Cationic Assembly of Metal Complex Aggregates: Structural Diversity, Solution Stability, and Magnetic Properties
Xiang Lin; Dan M. J. Doble; Alexander J. Blake; Andrew Harrison; Claire Wilson; Martin Schröder; Journal of the American Chemical Society 125 (2003) 9476–9483; doi:10.1021/ja0341438

data_4114019
_publ_section_title
;
 Cationic Assembly of Metal Complex Aggregates: Structural Diversity,
 Solution Stability, and Magnetic Properties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9476
_journal_page_last               9483
_journal_paper_doi               10.1021/ja0341438
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety
;
{(Na3 Li2 O) [Ni(C9 H12 N2 O4)]8 (B F4)0.86 (C H4 O)1.14} 
(B F4)2.14 (C H4 O)2.25 (C4 H10 O)0.75
;
_chemical_formula_sum            'C78 H112 B3 F12 Li2 N16 Na3 Ni8 O37.5'
_chemical_formula_weight         2686.80
_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                81.121(2)
_cell_angle_beta                 66.353(2)
_cell_angle_gamma                67.274(2)
_cell_formula_units_Z            2
_cell_length_a                   16.764(2)
_cell_length_b                   20.095(2)
_cell_length_c                   20.617(2)
_cell_measurement_reflns_used    4635
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      2.2
_cell_volume                     5868.2(11)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            69857
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             2756
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.35
_refine_diff_density_min         -1.09
_refine_diff_density_rms         0.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1520
_refine_ls_number_reflns         22954
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1099P)^2^+16.8549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.1926
_reflns_number_gt                17926
_reflns_number_total             27216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0341438si20030113_122949_08.cif
_cod_data_source_block           linibf_complex8
_cod_original_formula_sum        'C78 H112 B3 F12 Li2 N16 Na3 Ni8 O37.50'
_cod_database_code               4114019