Four Ni^II^ complexes with the new cyclam‒methylimidazole ligand 1-[(1-methyl-1<i>H</i>-imidazol-2-yl)methyl]-1,4,8,11-tetraazacyclotetradecane
De Candia, Ariel G.; Molnar, Matias; Slep, Leonardo D.; Baggio, Ricardo; Acta Crystallographica Section C 68 (2012) m121–m126; doi:10.1107/S0108270112014904

data_2018474
_publ_section_title
;
 Four Ni^II^ complexes with the new cyclam--methylimidazole ligand
 1-[(1-methyl-1<i>H</i>-imidazol-2-yl)methyl]-1,4,8,11-tetraazacyclotetradecane
;
_journal_coeditor_code           FA3274
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m121
_journal_page_last               m126
_journal_paper_doi               10.1107/S0108270112014904
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni (C20 H36 N6)] (Cl O4)2 , 0.24H2 O'
_chemical_formula_moiety         'C20 H36 N8 Ni 2+, 2(Cl O4 -), 0.24(H2 O)'
_chemical_formula_sum            'C20 H36.48 Cl2 N8 Ni O8.24'
_chemical_formula_weight         650.50
_chemical_name_systematic
;
<i>cis</i>-{1,8-bis[(1-methyl-1<i>H</i>-imidazol-2-yl)methyl]-1,4,8,11-
tetraazacyclotetradecane}nickel(II) bis(perchlorate) 0.24-hydrate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.7285(12)
_cell_length_b                   19.2330(18)
_cell_length_c                   21.171(2)
_cell_measurement_reflns_used    4665
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      2.02
_cell_volume                     5590.0(9)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Oxford Gemini CCD S Ultra'
_diffrn_measurement_method       '\w scans, thick slices'
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40257
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2009)'
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2723
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         5489
_refine_ls_number_restraints     934
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0670P)^2^+4.2236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1512
_reflns_number_gt                3936
_reflns_number_total             5489
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3274.cif
_cod_data_source_block           4
_cod_original_cell_volume        5589.9(9)
_cod_original_formula_sum        'C20 H36.48 Cl2 N8 Ni O8.24 '
_cod_database_code               2018474
_cod_database_fobs_code          2018474