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_2018473
_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 (Cl O4) (C15 H30 N6)] Cl O4'
_chemical_formula_moiety         'C15 H30 Cl N6  Ni O4 +, Cl O4 -'
_chemical_formula_sum            'C15 H30 Cl2 N6 Ni O8'
_chemical_formula_weight         552.06
_chemical_name_systematic
;
<i>trans</i>-{1-[(1-methyl-1<i>H</i>-imidazol-2-yl)methyl]-1,4,8,11-
tetraazacyclotetradecane}(perchlorato)nickel(II) perchlorate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 92.849(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.665(5)
_cell_length_b                   9.696(5)
_cell_length_c                   13.936(5)
_cell_measurement_reflns_used    3890
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      3.67
_cell_volume                     2249.0(16)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23451
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    1.155
_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    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4403
_refine_ls_number_restraints     732
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0541P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                2878
_reflns_number_total             4403
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3274.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018473
_cod_database_fobs_code          2018473