Anion Template Effect on the Self-Assembly and Interconversion of Metallacyclophanes
Cristian Saul Campos-Fernández; Brandi L. Schottel; Helen T. Chifotides; Jitendra K. Bera; John Bacsa; John M. Koomen; David H. Russell; Kim R. Dunbar; Journal of the American Chemical Society 127 (2005) 12909–12923; doi:10.1021/ja052108q

data_4111910
_publ_contact_author_address
; 
Department of Chemistry
Texas A&M University
PO Box 30012 
College Station 
Texas 77842-3012 
USA
;
_publ_contact_author_email       dunbar@mail.chem.tamu.edu
_publ_contact_author_fax         (979)8457177
_publ_contact_author_name        'Kim Dunbar'
_publ_contact_author_phone       (979)8621485
_publ_section_title
;
 Anion Template Effect on the Self-Assembly and Interconversion of
 Metallacyclophanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12909
_journal_page_last               12923
_journal_paper_doi               10.1021/ja052108q
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C64 H56 N32 Ni4, 7(F6 Sb), I'
_chemical_formula_sum            'C64 H56 F42 I N32 Ni4 Sb7'
_chemical_formula_weight         3285.40
_chemical_name_common            '[Ni4(bptz)4(CH3CN)8][SbF6]7[I]'
_space_group_IT_number           23
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      23
_symmetry_space_group_name_Hall  'I 2 2'
_symmetry_space_group_name_H-M   'I 2 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'October 5 2004'
_audit_creation_method
;
SHELXL-97, PLATON, and text editor
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.145(4)
_cell_length_b                   14.925(3)
_cell_length_c                   22.529(4)
_cell_measurement_reflns_used    4389
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.023
_cell_measurement_theta_min      2.028
_cell_volume                     6101(2)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'SMART 1K CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22697
_diffrn_reflns_theta_full        27.13
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    2.488
_exptl_absorpt_correction_T_max  0.5078
_exptl_absorpt_correction_T_min  0.2181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       block
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.68
_exptl_crystal_size_min          0.31
_refine_diff_density_max         2.076
_refine_diff_density_min         -2.616
_refine_diff_density_rms         0.207
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881.
The data indicated merohedral twinning by inversion. The structure 
was refined with an inversion twin law.  Although the absolute structure
parameter is zero, the twin populations refined to 50% and no definitive
statement about the absolute structure can be made.

;
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6678
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0655
_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^)+(0.1214P)^2^+54.1848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1694
_reflns_number_gt                5689
_reflns_number_total             6678
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja052108qsi20050419_040417.cif
_cod_data_source_block           GLOBAL
_cod_database_code               4111910