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_4111913
_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
'C50 H35 Br7 N25 Ni4, 2.5(C7 H8), 2(C2 H3 N), Br3'
_chemical_formula_sum            'C71.5 H61 Br10 N27 Ni4'
_chemical_formula_weight         2332.41
_chemical_name_common            '[Ni4(bptz)4Br7(CH3CN)Br3]\y2CH3CN\y2.5C6H5CH3'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_date             'October 28 2004'
_audit_creation_method
;
SHELXL-97, PLATON, and text editor.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.45(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.197(3)
_cell_length_b                   27.700(6)
_cell_length_c                   23.557(5)
_cell_measurement_reflns_used    2531
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      19.9
_cell_measurement_theta_min      2.21
_cell_volume                     8469(3)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.1422
_diffrn_reflns_av_sigmaI/netI    0.2120
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43302
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    5.652
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.1900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_description       plate
_exptl_crystal_F_000             4564
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.380
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       0.00003(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   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         15992
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.2090
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.2046
_reflns_number_gt                6525
_reflns_number_total             15992
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja052108qsi20050419_040601.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4111913