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_4114020
_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_sum            'C58.85 H91.4 Cl2 Li4 N12 Ni6 O37.85'
_chemical_formula_weight         2023.56
_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                 96.125(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.222(2)
_cell_length_b                   32.678(5)
_cell_length_c                   20.272(3)
_cell_measurement_reflns_used    5999
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.7
_cell_measurement_theta_min      2.3
_cell_volume                     8709(2)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.071
_diffrn_reflns_av_sigmaI/netI    0.118
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42903
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       column
_exptl_crystal_F_000             4181
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.19
_refine_diff_density_min         -0.83
_refine_diff_density_rms         0.21
_refine_ls_extinction_coef       0.0029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1173
_refine_ls_number_reflns         16884
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.176P)^2^+16.452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2773
_refine_ls_wR_factor_ref         0.3024
_reflns_number_gt                9325
_reflns_number_total             20284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0341438si20030113_122949_09.cif
_cod_data_source_block           nilil6_complex9
_cod_original_cell_volume        8709(3)
_cod_original_formula_sum        'C58.85 H91.40 Cl2 Li4 N12 Ni6 O37.85'
_cod_database_code               4114020