Synthesis, structure and electrochemistry of isomeric nickel(II) complexes of a [9]ane fused cyclam macrotricycle: evidence for a stable trans-IV and a redox induced rearrangement in a trans-I conformation.
McAuley, Alex; Subramanian, S.; Barclay, T.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 9956–9961; doi:10.1039/c0dt00550a

data_7026626
_publ_section_title
;
 Synthesis, structure and electrochemistry of isomeric nickel(II)
 complexes of a [9]ane fused cyclam macrotricycle: evidence for a stable
 trans-IV and a redox induced rearrangement in a trans-I conformation.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9956
_journal_page_last               9961
_journal_paper_doi               10.1039/c0dt00550a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         trans-[Ni(C18H36N4S2)](ClO4)2
_chemical_formula_sum            'C18 H36 Cl2 N4 Ni O8 S2'
_chemical_formula_weight         630.24
_chemical_name_common            trans-(Ni((9)N4S2))diperchlorate
_chemical_name_systematic        trans-[Ni([9]N4S2)]diperchlorate
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 129.657(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.384(9)
_cell_length_b                   10.118(2)
_cell_length_c                   14.300(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      4
_cell_volume                     2493.4(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  smart1000
_diffrn_measurement_method       omega
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6350
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            lightpink
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    na
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.093
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+9.5812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1525
_reflns_number_gt                1713
_reflns_number_total             2193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00550a.txt
_cod_data_source_block           tNi9N4S2
_cod_original_cell_volume        2493.3(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7026626