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_7026625
_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         cis-[Ni(C18H36N4S2)]Cl24H2O
_chemical_formula_sum            'C18 H44 Cl2 N4 Ni O4 S2'
_chemical_formula_weight         574.30
_chemical_name_common            cis-(C18H36N4S2)Ni(ii)dichloridetetrahydrate
_chemical_name_systematic        cis-(C18H36N4S2)Ni(II)dichloridetetrahydrate
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.450(3)
_cell_length_b                   12.188(2)
_cell_length_c                   11.897(2)
_cell_measurement_reflns_used    488
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      4
_cell_volume                     2530.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12895
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    na
_exptl_crystal_description       na
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.496(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4440
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0476P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                3770
_reflns_number_total             4440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00550a.txt
_cod_data_source_block           1_database_code_depnum_ccdc_archive
_cod_original_cell_volume        2530.3(8)
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               7026625