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_4114022
_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            'C84 H124 Cl3 N18 Na4 Ni9 O53.5'
_chemical_formula_weight         2968.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens
'CH3 found in delta-F, CH2 placed geometrically, solvent Hs not found'
_atom_sites_solution_primary     'Heavy atom methods'
_atom_sites_solution_secondary   'difference Fourier synthesis'
_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                   17.008(2)
_cell_length_b                   17.008(2)
_cell_length_c                   25.054(5)
_cell_measurement_reflns_used    220
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      0
_cell_volume                     6276.5(16)
_computing_cell_refinement       'IPDS (1995)'
_computing_data_collection       'IPDS (1995)'
_computing_data_reduction        'IPDS (1995)'
_computing_molecular_graphics    'SHELXTL/PC (Version 5.03, Sheldrick, 1994)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997); PLATON (Spek, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe Imaging plate diffractometer system'
_diffrn_measurement_method       'area detector'
_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  0.117
_diffrn_reflns_av_sigmaI/netI    0.093
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24548
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.490
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(HABITUS; Herrendorf, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_F_000             3058
_refine_diff_density_max         1.02
_refine_diff_density_min         -1.22
_refine_diff_density_rms         0.14
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    'riding models'
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         10027
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.104
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.138P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.179
_refine_ls_wR_factor_ref         0.199
_reflns_number_gt                7728
_reflns_number_total             10027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0341438si20030113_122949_11.cif
_cod_data_source_block           NIXCLU_Compound_11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.138P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.138P)^2^] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6276.8(18)
_cod_original_formula_sum        'C84 H124 Cl3 N18 Na4 Ni9 O53.50'
_cod_database_code               4114022