Synthesis and hydrolysis of cis-octahedral nickel(II) complexes with C-racemic tetraaza macrocycles bearing two imidate ester pendant arms
Soonmoo Bang; Nahee Kim; Shin-Geol Kang; Jong Hwa Jeong; Inorganica Chimica Acta 392 (2012) 184–191; doi:10.1016/j.ica.2012.05.035

data_1512479
_publ_section_title
;
 Synthesis and hydrolysis of cis-octahedral nickel(II) complexes with
 C-racemic tetraaza macrocycles bearing two imidate ester pendant arms
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              184
_journal_page_last               191
_journal_paper_doi               10.1016/j.ica.2012.05.035
_journal_volume                  392
_journal_year                    2012
_chemical_formula_moiety         'C24 H50 N6 Ni O2, 2(Cl O4)'
_chemical_formula_sum            'C24 H50 Cl2 N6 Ni O10'
_chemical_formula_weight         712.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 119.74(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   36.748(3)
_cell_length_b                   20.6365(9)
_cell_length_c                   19.503(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.82
_cell_measurement_theta_min      9.36
_cell_volume                     12842(11)
_computing_cell_refinement       'CAD4 software'
_computing_data_collection       'CAD4 software (Enraf-Nonius. 1989)'
_computing_data_reduction        'XCAD (McArdle, 1999)'
_computing_molecular_graphics    'ORTEPIII for windows (McArdle, 1995)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 4-circle diffractometer'
_diffrn_measurement_method       \w/2\q
_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  0.0075
_diffrn_reflns_av_sigmaI/netI    0.1145
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12805
_diffrn_reflns_theta_full        25.47
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         1.89
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_process_details   '(ABSCALC; McArdle & Daly, 1999)'
_exptl_crystal_colour            pale-bluepurple
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6048
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         11931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.1449
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0940P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1610
_reflns_number_gt                5712
_reflns_number_total             11931
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ICA-2012-392-184-191-1.cif
_cod_data_source_block           k07b
_cod_original_cell_volume        12841(11)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C24 H50 Cl2 N6 Ni O10 '
_cod_database_code               1512479